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WORKSHOP #6
Vaping:
What You Didn’t Know About Electronic Cigarettes and Why You Should Care
SOFT 2016
Dallas, TX
Monday, October 17, 2016
Chairs:
Michelle Peace and Justin Poklis
Workshop #6 Vaping: What You Didn’t Know About Electronic Cigarettes
and Why You Should Care
October 17, 2016
Agenda:
1:30 pm - 1:45 pm Introductions Michelle R. Peace
1:45 pm - 2:45 pm Basic Mechanisms and Efficacy of Aerosols in Drug Delivery Richard Dalby
2:45 pm - 3:30 pm The E-Cig Evolution: Use, Operation, and Manipulation Michelle R. Peace
3:30 pm - 4:00 pm Afternoon Break
4:00 pm - 4:45 pm Analysis of the E-Cigs and E-Liquids Justin L. Poklis
4:45 pm - 5:30 pm Case Examples Justin Victoria and Juan Colon
Richard N. Dalby, Ph.D. University of Maryland School of Pharmacy Department of Pharmaceutical Sciences
20 N. Pine Street, Baltimore, MD 21201 (410) 706-3245
[email protected] www.pharmacy.umaryland.edu/faculty/rdalby
Dr. Richard Dalby is a Professor in the Department of Pharmaceutical
Sciences at the University of Maryland, School of Pharmacy. He holds a Bachelor
of Pharmacy degree (1983) from Nottingham University in England, and a Ph.D.
in Pharmaceutical Sciences from the University of Kentucky (1988).
Dr. Dalby's aerosol research, which encompasses novel pulmonary and
nasal formulation development, device design, product testing and human
factors, is founded on his Ph.D. work on sustained release metered dose inhalers
and industrial experience as a Formulation Scientist. He has published more than
50 peer reviewed papers and over 130 abstracts related to aerosol technology,
authored several book chapters, and spoken at many national and
international meetings. He is an inventor on five patents concerned with novel
inhaler formulations, a reviewer for several international journals and a frequent
industrial and FDA invited speaker. Dr. Dalby has extensive experience as an
expert witness in cases involving inhaled drugs – mostly he testifies in Intellectual
Property cases rather than the exciting stuff you guys get involved with!
Dr. Dalby is the director of the Inhalation Aerosol Technology Workshop
which is taught at company facilities worldwide, and co-organizer and editor of
Respiratory Drug Delivery (RDD®), and its spin-offs, RDD Europe and RDD Asia.
RDD meetings attract 450-750 internationally known scientists, regulators and
business professionals active in nasal and pulmonary drug delivery.
Dr. Dalby is a Fellow of the American Association of Pharmaceutical
Scientists. He is generally good-natured but a natural trouble causer.
Basic Mechanism & Efficacy of Aerosols in Drug Delivery
Richard Dalby, Ph.D.University of Maryland School of Pharmacy
SOFT Annual Meeting, October 17, 2016
Financial Disclosures• No manufacturers of products listed or discussed within this
presentation provided any financial support for this project• I have no actual or potential conflict of interest in relation to
this workshop presentation
Educational Objective• Understand the mechanism and advantage of aerosols as a
drug delivery system
Inhaled Drugs• Ancient civilizations, current
smokers and drug abusers knowthat inhaled drugs:
– Act quickly
– Minimize the dose required
– Are non-invasive
– Are systemically absorbed
• Scientists later discovered/inferredthat inhaled drugs:
– Minimize side effects throughlocal delivery
– Avoid hepatic first-pass metabolism
Cigarette Smoke (0.3μm)
• The aerosol is formedby condensation ofheated vapor intodroplets.
• This is a “stable” liquidaerosol because thedroplets don’t quicklyfall under the influenceof gravity.
Pressurized Sprays (1-5 μm)
Evaporation
Deceleration
Propellant evaporation
Drug particles inpropellant droplets
Aggregated drugparticles
Device Design ConstraintsPhysiology & Disease
Patient Attributes
Scientific & Engineering Feasibility
Cost vs. Therapeutic Outcome
Flo
w
Tidalvolume
Inspiratorycapacity
pMDI / DPINebulizer
Normal Asthma
• Portable• Remaining product is
uncontaminated• Tamper-resistant• Protects drug from
Light, O2 and H2O• Multiple dose• Accurate dosing• Inexpensive technology• Apparently Easy to Use
Pressurized Metered Dose Inhalers
Pressurized Metered Dose Inhaler
• Propellant
• Surfactant and/or co-solvent
• Drug (dissolved or suspended)
Typical pMDI Spray
Droplet evaporation& deceleration
Proventil HFAMicrocrystalline suspension of albuterol sulfate in HFA-134a, ethanol and oleic acid.
200 inhalations.
Each actuation delivers 120 mcg albuterol sulfate, USP from the valve
Each actuation delivers 108 mcg albuterol sulfate, USP from the mouthpiece (equivalent to 90 mcg of albuterol base from the mouthpiece).
Merck US package insert
Patient Technique Problems
• Fires during exhalation
• Fires before inspiration
• Fires at end of inspiration
• Firing stopped inhalation
• Firing into mouth whileinhaling through the nose
• Multiple actuations during a single inhalation
• Failure to fire MDI due to infirmity
• Inappropriate inhaled flow rate
Compton, G.K. Eur. J. of Resp Disease, Suppl. 119, 63 (1982)
Other RespiratoryDrug Delivery Platforms
Disadvantages of pMDIs
• Expensive & environmentallyquestionable propellants
• Substantial training needed
• Inappropriate patient use
Air Jet Nebulizers
• Aqueous base
• Drug is usuallydissolved
20mm Tconnector
Sprayorifice
Compressedair
Baffle
Operation of anAir-Jet Nebulizer
• Liquid Shearing– Primary droplets are recirculated
– Satellite droplets are inhaled
• Jet design, orifice diameter baffle placement
• Gas pressure, density and flow rate
• Concentration, surface tension and viscosity ofdrug solution
• Solution cools during use
Ultrasonic Nebulizers
• Ceramic Piezo element bonded tometal mesh vibrates in response toalternating voltage
• Goal is maximum displacement withminimum voltage
• Higher frequency causes higherdroplet output but can generate heator shear
• Droplets are produced by extrusionthrough a mesh
Breath Actuated Nebulizers
Aero Eclipse II (Monaghan)
Aerogen Aeroneb Pro
Controlling Aerosol Generation
• Microprocessor controlled aerosol generation• Three breath rolling average breathing tracking• High efficiency
Time
Volume
I-neb AAD® System (Philips)
The Continued Appeal ofAtomizing Aqueous Solutions
• Device can be developed independentlyof drug formulation
• Formulations are relatively easy tomanufacture
• Potentially useful with fragile biologicalmolecules
• No environmental concerns
• Drug delivered in asingle inhalation
• Reservoir holds up to200 doses in a hand-held unit
• Less contaminationproblems thanconventional nebulizers
• Drug solutionspecificto device
Soft Mist Inhaler
Respimat®
(Mechanical break-up)
• Automatic coordinationbetween dose delivery andinhalation
• No propellants
• Potential drug stabilityadvantages
• High dose carrying capacity
Dry Powder Inhalers
DPI Particle Agglomerate Designs to Facilitate Initial Powder Flow and Subsequent Deaggregation
Shear applicationresulting fromairflow through
the inhaler
Drug particle
Carrier particle
Particle state during powder filling and storage
Particle state when airflow occurs
Drug-carrier aggregates
Drug only aggregates
A micronized or spraydried powder is…
Inhaled
Deaggregated
Entrained
Metered
…using energy from onlythe patient’s inhalation
Passive Dry Powder Inhalers
Turbuhaler®
Powder in Capsules
Potentially tricky reloading step required for every dose
Capsule shattering or crushing during piercing
Aerolizer® - NovartisForadil® (formoterolfumarate)
HandiHaler® - BISpiriva® (tiotropium)
• Complex devicespotentially difficult to fill
• Blister handling makesdevice relatively bulky
Powder in Blisters
Diskus®
Ellipta®
Starhaler®
Powder in Cartridge
Dreamboat®
Powder in Reservoir
• Suboptimal dosingreproducibility
• Orientation sensitive
• Moisture sensitive
Turbuhaler®
A powder is…
Inhaled
Deaggregated
Entrained
Metered
…using energy from apatient-independent source
Active Dry Powder Inhalers
Exubera®
Staccato® (Thermal condensation aerosol)
(1) Battery & electronic controls
(2) “Juice” reservoir & mouthpiece
(3) Vaporization chamber
Anatomy of a Generic E-cigarette
Aerosol exits
mouthpiece
Battery +Connections -
Wick
Vaporization chamber
Generic Vaporization Chamber
Ambient air inlets
Juice
Reservoir
Heating coil
Condensation aerosol out
Maximum reactivity is expected where the “juice”, air and heating coil are in close proximity
Wick (Sn, Pb, Fe, Cu,Zn, Co & Ni)
Ambient air (No metals)
Heating coil(Sn, Fe, Cu & Zn)
Reservoir & mouthpiece components
(Pb, Fe, Cu, Zn, Co & Ni)
Tobacco & Menthol “Juice” (No metals)
Sources of Metals in KangerTech® EVOD
Potentially Bioactive or Toxic Metals in E-cigarette Materials of ConstructionSarah L. J. Michel, Maureen A. Kane, Abraham Schneider, Richard N. Dalby, Geoffrey Shimberg, Tao Ma and Thao Vo (in preparation)
The Upper Respiratory Tract
Goblet cell(mucus)
Cilia
Mucus layer
• Target for bronchodilators and steroids(site of maximum airway resistance)
• Target for antiinfectives (viscous mucus)
The Lower Respiratory Tract• Target for systemically acting drugs
(site of maximum absorption)
– Agitation (loxapine, Adasuve®)
– Diabetes (Rapid acting insulin Afrezza®)
Alveolar airspace
Alveolar cell
Capillary containingred blood cells
Beta-2 agonists
Short Acting (SABA)
Albuterol(Proventil®)
Long Acting (LABA)
Salmeterol(Serevent®)
Fast acting LABA
Formoterol
Anticholinergics Ipratropium bromide
(Atrovent®) Tiotropium bromide
(Spiriva®)
Glucocorticosteroids Beclomethasone dipropionate
(Beclovent®) Budesonide (Pulmicort®)
Fluticasone (Flovent®)
Antiinflammatories Cromolyn sodium (Intal®)
Double and Triple Combinations– Salbutamol & fluticasone (Advair®)– Formoterol & fluticasone (Flutiform®)– Long-acting anti-cholinergic
bronchodilator, long-acting beta-agonist bronchodilator &corticosteroid
Inhaled Locally Acting Drugs
Inhaled Systemically Acting Drugs• Late-stage development
– Agitation (loxapine, Adasuve®)
– Type II diabetes (rapid acting insulin, Afrezza®)
• Early development– Pain management (fentanyl, morphine)
– Hormones
– siRNA
– Vaccines
What Determines Where Inhaled Particles Deposit?
• Inhaled Particles– Size
– Shape, Density, Charge, Hygroscopicity
• Patient– Lung Anatomy
– Disease State
– Technique
– Breathing Pattern
• Aerosol Generation Device– Principle and Design Features
(1) Ambient air enters e-cigarette (2) Aerosol condensate (“smoke”)
exits e-cigarette
Capturing Toxicants in theAerosol Condensate
(4) Aerosol condensate trapped in cell growth medium using bubbler
(3) Breathing simulator mimics the “draw” on an e-cigarette causing
aerosol generation
Rusty makes his move
The Far Side, Gary Larson
Thanks for Listening
Questions?
Michelle R. Peace, Ph.D. Virginia Commonwealth University Department of Forensic Science
1015 Floyd Ave, Richmond, VA 23284 804.828.8420
Dr. Peace received her B.A. in Chemistry from Wittenberg University, a
Master of Forensic Science from George Washington University, and her Ph.D.
from the Medical College of Virginia at Virginia Commonwealth University
(VCU). The focus of her doctoral work was to study entomological evidence as
an alternative matrix for toxicological analyses.
Dr. Peace currently serves as the Associate Chair for the Department of
Forensic Science at VCU (FEPAC-accredited). She is one of the founding faculty
for the Department, and has served as Associate Chair more than 4 years. She
also served as the Interim Chair for 4 years, expanding the faculty, physical
space, research initiatives for the Department. Dr. Peace has also served as a
manager in a private SAMHSA-accredited forensic urine drug testing laboratory
and worked as a scientist for Procter & Gamble, where she holds 3 patents.
Dr. Peace served on the Scientific Working Group for Forensic Toxicology
(SWGTOX) for 4 years, is a member of the Society of Forensic Toxicologists (SOFT)
and is its current Treasurer, and is a member of the Toxicology Section of the
American Academy of Forensic Sciences. She has conducted continuing
education workshops for professionals nationwide and has developed
workshops for primary and secondary education and a community
engagement enterprise to address STEM education in middle schools.
Dr. Peace is currently the PI for an NIJ grant studying the efficacy of
electronic cigarettes and has served as the PI as a sub-grantee for the Forensic
Technology Center of Excellence, in which she managed a complex evaluation
of crime scene scanners, collaborating with 4 law enforcement agencies.
CHARACTERIZATION AND ABUSE OF ELECTRONIC CIGARETTES:
THE EFFICACY OF “PERSONAL VAPORIZERS” AS AN ILLICIT DRUG DELIVERY SYSTEM
PI: Michelle Peace, Ph.D., Department of Forensic Science
Co-PIs: Alphonse Poklis, PathologyJustin Poklis, Pharmacology and ToxicologyJoseph Turner, Chemistry
FINANCIAL DISCLOSURES
• No product or instrument manufacturers listed or discussed within this presentation provided any financial support for this project
• The presenter has no actual or potential conflict of interest in relation to this workshop presentation
• Characterization and Abuse of Electronic Cigarettes: The Efficacy of“Personal Vaporizers” as an Illicit Drug Delivery System is supported by Award No. 2014-R2-CX-K010, awarded by the National Institute of Justice, Office of Justice Programs, U.S. Department of Justice. The opinions, findings, and conclusions or recommendations expressed in this publication/program/exhibition are those of the author(s) and do not necessarily reflect those of the Department of Justice.
• Some of the analytical research in this project have also been supported by the National Institute of Health Grant No. P30DA033934. Opinions, findings, conclusions, and recommendations are those of the authors and also do not necessarily reflect those of the NIH.
THE E-CIG EVOLUTION, A LONG HISTORY:USE, OPERATION, AND MANIPULATION
HISTORY OF ELECTRONIC CIGARETTES
1927
1930
1965
2001
2003
2004
2006
2007
2009-Present
1927• Electronic Vaporizers 1st
Developed• Joseph Robinson
1927
1930
1965
2001
2003
2004
2006
2007
2009-Present
1930• Patent Approved
• Electronic Vaporizers
• Joseph Robinson
HISTORY OF ELECTRONIC CIGARETTES
1965• Patent Approved
• Smokeless non-tobacco cigarette
• Herbert A. Gilbert• “…to provide a safe and
harmless means for smoking by replacing burning tobacco with heated, moist, flavored air…”
HISTORY OF ELECTRONIC CIGARETTES
1927
1930
1965
2001
2003
2004
2006
2007
2009-Present
1927
1930
1965
2001
2003
2004
2006
2007
2009-Present
2001• Hon Lik - desire to
quit smoking
HISTORY OF ELECTRONIC CIGARETTES
1927
1930
1965
2001
2003
2004
2006
2007
2009-Present
2003• Hon Lik’s father
passed away• Lung cancer
HISTORY OF ELECTRONIC CIGARETTES
1927
1930
1965
2001
2003
2004
2006
2007
2009-Present
2004• Patent approved
• Hon Lik• Electronic
Atomization Cigarette
HISTORY OF ELECTRONIC CIGARETTES
2006• Electronic
cigarettes on the market in Europe
1927
1930
1965
2001
2003
2004
2006
2007
2009-Present
HISTORY OF ELECTRONIC CIGARETTES
2007• Electronic
cigarettes on the market in the United States
HISTORY OF ELECTRONIC CIGARETTES
1927
1930
1965
2001
2003
2004
2006
2007
2009-Present
2009-Present• Trouble began to
ensue in the USA in 2009• FDA study• FDA ban on import• Proposed regulation
• Electronic cigarette industry continues expansion
HISTORY OF ELECTRONIC CIGARETTES
1927
1930
1965
2001
2003
2004
2006
2007
2009-Present
May 05, 2016• FDA swept e-cigs under
regulatory authority• Includes other “electronic
products”• Includes cigars, pipe
tobacco, hookah tobacco
• By 2018, products must contain warning statement
HISTORY OF ELECTRONIC CIGARETTES
1927
1930
1965
2001
2003
2004
2006
2007
2009-Present
ELECTRONIC CIGARETTES
E-CIGS ON THE MARKET
First Generation – “Ciga-like”
looks like real cigarettes simplest make-up (battery, coil,
and filling) low single voltage can contain a cartomizer appeal to visual users trying to
quit traditional cigarettes
Second Generation – “Mid-size” looks like a pen larger than cigalikes and are
more customizable commonly called a clearomizer rechargeable battery and
refillable tank decreases cost
E-CIGS ON THE MARKET
Third Generation – “Advanced Personal Vaporizers”
stronger batteries and various settings
rebuildable atomizer smoked by advanced vapers
because of the endless modification possibilities
E-CIGS – MORE LINGO
ATOMIZER • Everything is an atomizer of some form• Coil + wicking device + battery*
CARTOMIZER • Single wire surrounded by a poly-fill wick
CLEAROMIZER • Tank + Atomizer
E-CIGARETTES IN THE MEDIA
E-CIGARETTES AND CRIME• E-cigarettes have become a popular method for abuse of
drugs• Convenient and public “clandestine” use • Marketing directed toward minors and young adults
“You can get away with vaporizing methamphetamine at work this way... some places let you smoke e-cigs inside.” –bluelight.org
E-CIGARETTES AND CRIME• E-cigarettes have become a popular method for abuse of
drugs• Lack of regulation led to ease of purchase for minors
E-CIGARETTES IN THE MEDIA
E-CIGARETTES IN THE MEDIA
E-CIGARETTES IN THE (SOCIAL)MEDIA
E-CIGARETTES IN THE (SOCIAL)MEDIA
#VapeMJ#CloudChase
#Weed#Vacuum
#BlueMeth#Heisenberg
www.vine.co
First Generation E-Cig Third Generation E-Cig
E-LIQUIDS IN POISON CONTROL CENTERS
https://aapcc.s3.amazonaws.com/files/library/E-cig__Nicotine_Web_Data_through_12.2015.pdf
American Association of Poison Control CentersE-Cigarette Device and Liquid Nicotine Reported Exposures
2011 2012 2013 2014 2015 2016
[VALUE] [VALUE]
1543
3783
3067
1038
1 2 3 4 5 6
Reported Cases
E-CIGS POSTMORTEM: ?• Tooth loss• Broken neck• Coma• Severe burns
Naples, FL
UK
E-CIGS POSTMORTEM:
Betty C. Chen, Steven B. Bright, Amit Raj Trivedi & Matthew Valento (2015) Death following intentional ingestion of e-liquid, Clinical Toxicology, 53:9, 914-916, DOI: 10.3109/15563650.2015.1090579
Death Following Intentional Ingestion of E-liquid• 24yo female, unresponsive, pulseless• Intentional suicidal ingestion (suicide note)
• Partially ingested bottle of whiskey• 2 empty 15ml vials of concentrated nicotine (100mg/ml)• Prescription meds had appropriate pill counts
• Arrival in ED:• BP: 74/53; Pulse: 106bpm; Respiration: 14 breaths/min• Pupils fixed and dilated
• Admission to ICU:• Myoclonic jerking• Absence of corneal, gag, and cough reflexes• Anoxic brain injury by MRI
• Toxicology:• GC-MS screening: Positive for nicotine, cotinine, and Rx• LC-MS3 : Plasma nicotine and cotinine >1000ng/ml
• E-liquid bottles were not tested• Died 3d post-ingestion
E-CIGS POSTMORTEM:
Gundong You, Jongsook Rhee, Yuran Park, Sunhye Park (2016), Determination of Nicotine, Continine, and Trans 3’-Hydroxycotinine using LC/MS/MS in Forensic Samples of a Nicotine Fatal Case by Oral Ingestion of e-cigarette Liquid, J Forensic Science, 61(4), 914-916, DOI: 10.1111/1556-4029.13083
Death Following Ingestion of E-liquid• 39yo male found dead on floor of dental clinic• E-cigarette and LIQ e-liquid found near body• Analyses performed on liquid, heart blood, peripheral blood,
and gastric contents (106g)• Toxicology:
• Heart blood: 87.2 mg/L nicotine, 1.4 mg/L cotinine• Peripheral blood: 85.2 mg/L nicotine, 1.1 mg/L cotinine• Gastric contents: 6735 mg/kg nicotine• No report of concentration of nicotine in eliquid
• Conclusion: oral ingestion • Will promote the danger of e-liquid ingestion
E-CIGS POSTMORTEM:
Stephen Thorton, Lisa Oller, Tama Sawyer (2014), Fatal Intravenous Injection of ENDS Refilling Solution, J Med Toxicol 10, 202-204, DOI: 10.1007/s13181-014-0380-9
Death Following Injection of E-liquid• 29yo male found unresponsive by family• History of depression, not taking Rx medications• Found with a suicide note indicating injection of e-liquid• Wife claimed he was using e-cigs to stop smoking• EMS: defibrillated twice, intubated, given atropine, sodium
sodium bicarb, and lidocaine• Hospital: pupils fixed, tonic/clonic seizures, 125 bpm heart
• Put in therapeutic hypothermia• Never regained consciousness• Autopsy not performed
• Serum drug screen:• Positive for lidocaine, nicotine, cotinine• No amphetamines found• Serum nicotine/cotinine: 2000/2100 ng/ml
• Product not available for testing
FORENSIC TOXICOLOGY CONSULTATIONS
• Forensic Urine Drug Test Results• Development of a Nicotine Field Test• Blue Lotus Flower (apomorphine, nuciferine)
• Bee Juice (MDMB-Fubinaca)
• Overdose Deaths
ACKNOWLEDGEMENTS• Virginia Commonwealth University
• Department of Forensic Science • Joseph Turner, Ph.D., Chemistry• Justin Poklis, B.S., D-ABFT-FT, Pharm/Tox• Alphonse Poklis, Ph.D., F-ABFT, Pathology
• VCU Health• Carl Wolf, Ph.D.
• E-Cigarette Research Group:• Tyson Baird• Lori McLean• Karen Butler• Joseph Stone• Haley Mulder• Shelle Butler• Katilyn Brooks• Ivy Blue• Jesse Patterson• Rose Krakowiak• Laura McNew• Jimmy Stewart• Alex Dupont• Kaitlyn Forsythe• Jasmynne Royals
To watch a group of bees is to see a frenzy of different interestscoalesce into a single, clearthought.
–Jason Castro, Scientific American
IMAGE REFERENCEShttp://www.v2cigs.com/blog/wp-content/uploads/2013/10/1927-cig-patent.pnhttp://smokelesscigsource.com/e-cigarette-inventor-hon-lik-has-not-reaped-the-rewards/http://graphics8.nytimes.com/images/2013/10/09/business/ECIG/ECIG-articleLarge.jpg
http://cdn2.hubspot.net/hub/328747/file-500927646-jpg/blog-files/tobacco-expo-hits-vegas.jpg?t=1392134949000http://gaia.adage.com/images/bin/image/medium/Njoy_ad.jpg?1388688535http://www.inquisitr.com/264255/e-cigarettes-may-help-smokers-quit-improve-health/http://www.trappsclassichumidors.com/electronic-cigarette/electronic-cigarette-brands/http://shop.nhaler.com/Advanced-Personal-Vaporizers-Mods_c61.htm
http://www.kamry.cc/510-cartomizer-low-resistance.htmlhttp://www.kangeronline.com/products/t3s-clearomizer?variant=264612422http://www.onepoundeliquid.com/vape-hub/category/general-information/www.reddit.comwww.3bvape.comwww.dhgate.comwww.pradinr.comwww.myfoxatlanta.comMountiewire.com
https://www.rt.com/uk/220551-vape-dmt-electronic-cigarette/
http://www.fda.gov/TobaccoProducts/Labeling/ProductsIngredientsComponents/ucm491662.htmhttp://www.mirror.co.uk/news/uk-news/smoker-left-shocking-injuries-after-4435139http://archive.naplesnews.com/news/crime/exploding-e-cigarette-injures-woman-destroys-car-2caec708-5399-79a8-e053-0100007f6100-370300421.html
QUESTIONS?
www.flickr.com
Justin Poklis, BS, D-ABFT-FT Virginia Commonwealth University
Department of Pharmacology and Toxicology [email protected]
Justin Poklis received his BS in Chemistry from Virginia Commonwealth
University (VCU). He is currently the manager of operations for the Mass
Spectrometer Laboratory in the Pharmacology & Toxicology Department at
VCU. Prior to accepting his present position, he was a toxicologist at the Office
of the Chief Medical Examiner in North Carolina. He has also worked for the
Aerosol Research Group at VCU and for the Medical College of Virginia
Hospitals at VCU in the Clinical Toxicology Laboratories, known as the FIRM Lab.
He also worked at Scientific Testing Laboratories, a SAMSHA certified drug
testing facility. Mr. Poklis has contributed to over 50 peer review publication and
over 75 abstracts to scientific meetings. He is certified through the American
Board of Forensic Toxicology as a Diplomate in Forensic Toxicology.
Analysis of the
E-LiquidsJustin Poklis, BS, FTS-ABFT
Department of Pharmacology & Toxicology
Virginia Commonwealth University
Vaping: What You Didn’t Know About Electronic Cigarettes - And
Why You Should Care
No product or instrument manufacturers listed or discussed within this presentation provided any financial support for this project
The presenter has no actual or potential conflict of interest in relation to this workshop presentation
Financial Disclosures
E-liquids commonly comprised of
Propylene glycol and/or glycerin (humectants)
Various flavoring components
Traditional cigarette to candy
Active ingredients
Nicotine
Vitamins
Caffeine
Cannabinoids
Cannabidiol
Tetrahydrocannabinol
Any number of drugs/designer drugs
Electronic cigarette refill formulations or e-liquids
VCU Aerosol Research Group Liquid aerosol formulation comprising at least one thermally stable active ingredient
butalbital, lorazepam, ipratropium,
baclofen, morphine, scopolamine, buspirone, buprenorphine, triazolam, cyclobenzaprine, zolpidem
The liquid formulation - propylene glycol
one or more optional excipients
2008 US Patent No: 7,410,635 Aerosol formulations and aerosol delivery of scopolamine2009 US Patent No: 7,501,113 Aerosol formulations and aerosol delivery of buprenorphineUS Patent Application No: 20040151670 - Aerosol formulations and aerosol delivery of butalbital, lorazepam, ipratropium, baclofen, morphine and scopolamine
US Patent Application No: 20050079137 -Aerosol formulations and aerosol delivery of buspirone, buprenorphine, triazolam, cyclobenzaprine and zolpidem
Frank E. Blondino, Justin Poklis, Matthew Baker
The active ingredient
0.01 to 5% (weight)
Heated to generate an aerosol mass median aerodynamic diameter of < 3 µm
DARTTM parameters:Helium gas temp: 300 °C
Gas flow rate: 2 L/min
Electrode 1: 150 V
Electrode 2: 250 V
Discharge needle: 4000 V
AccuTOFTM Mass parameters:AccuTOF Detector: 2000 V
Orifice 1: 20, 30, 60, 90 V (Function Switching)
Orifice 2: 5V
Ion Guide: 400 V
Resolving power: 6000 FWHM
Ion Mode: Positive
Scan Range: 40-1000 Da
Mass Calibration: PEG 600
Direct Analysis in Real Time (DART)
Compound Adduct Formula Monoisotopic Mass Propylene Glycol -OH C3H7O 59.05Propylene Glycol +H C3H9O2 77.06Propylene Glycol 0 C3H12O2N 94.087Propylene Glycol x2 - OH C6H15O3 135.102Propylene Glycol x2 + H C6H17O4 153.113Propylene Glycol x2 + NH4 C6H20O4N 170.139Propylene Glycol x3 - OH C9H24O5 211.155Glycerin - OH C3H7O2 75.045Glycerin + H C3H9O3 93.055Glycerin 0 C3H12O3N 110.082Glycerin x2 + H C6H17O6 185.103Glycerin x2 + NH4 C6H20O6N 202.129Nicotine + H C10H15N2 163.124Nicotine x2 + H C20H29N4 325.239
DART – Propylene Glycol& Glycerin
Flavor Compound Flavor Characteristic Formula Monoisotopic MassBenzaldehyde Cherry C7H6O 107.0497Carvone Spearmint C10H14O 151.1123Vanillin Vanilla C8H8O3 153.0552Ethyl vanillin Vanilla C9H10O3 167.0715Isoamyl acetate Banana C7H14O2 131.1072Cinnamaldehyde Cinnamon C9H8O 133.0653Ethyl propionate Strawberry/Kiwi C5H10O2 103.0759Methyl anthranilate Grape C8H9NO2 152.0712Limonene Citrus C10H16 137.133Allyl hexanoate Pineapple C9H16O2 157.1229Methyl salicylate Wintergreen C8H8O3 153.0552Ethyl decadienoate Pear C12H20O2 197.1542Ethyl homovanillate Vanilla C11H14O4 211.097Diacetyl/Butanedione Butter C4H6O2 87.0446
DART – Typical Flavor Compound in E-liquids
75.0
43 G
lyce
rin
-OH
77.0
58 P
ropy
lene
Gly
col +
H
93.0
57 G
lyce
rin
+H
107.
049
Ben
zald
ehyd
e+
H
110.
084
Gly
ceri
n +
NH
4
163.
123
Nic
otin
e +
H
185.
102
Gly
ceri
n x2
+H
325.
240
Nic
otin
e x2
+H
0
50
100
Rel
. Int
ensi
ty
%
40 60 80 100 120 140 160 180 200 220 240 260 280 300 320 340
m/z
DART – Typical 20V Spectra of Nicotine E-liquid
153.
1115
Pro
pyle
ne G
lyco
l x2+
H
59.0
535
Pro
pyle
ne G
lyco
l -O
H
47.0
708
Eth
anol
+H
HPLC-MS/MS Quantitation of Nicotine
Instrumentation:Applied Biosystems 3200 Q TrapShimadzu SCL HPLC systemColumn:
Hypersil Gold® 3 X 50mm, 5 µ Mobile Phase:
10:90 10 mM ammonium formate: methanolIon transitions monitored:
Compound (m/z) CE (eV)Nicotine 163 > 130 30Nicotine 163 > 117 37Nicotine-d4 167 > 134 30
Instrument Parameters:Injection Volume: 10 µL
Flow Rate Pump A: 0.5 mL/min
Ionspray Voltage: 5000 V
Declustering Potential: 35 eV
Source Temp: 600 ºC
VapeWell Cheery - Nicotine-d4(IS) (Unknown) 167.0/134.0 amu - sample 45 of 105 from Data072114.wiff Area: 325515 counts Height: 37617 cps RT: 0.923 min
0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8Time, min
0.0
2000.0
4000.0
6000.0
8000.0
1.0e4
1.2e4
1.4e4
1.6e4
1.8e4
2.0e4
2.2e4
2.4e4
2.6e4
2.8e4
3.0e4
3.2e4
3.4e4
3.6e4
Intensity, cp
s
0.92
VapeWell Cheery - Nicotine (Unknown) 163.0/130.0 amu - sample 45 of 105 from Data072114.wiff Area: 1232221 counts Height: 146831 cps RT: 0.917 min
0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8Time, min
0.0
1.0e4
2.0e4
3.0e4
4.0e4
5.0e4
6.0e4
7.0e4
8.0e4
9.0e4
1.0e5
1.1e5
1.2e5
1.3e5
1.4e5
Intensity, cps
0.92
Nicotine-d4
Nicotine
Curtain Gas: 30 mL/min
Ion Source Gas 1: 50 mL/min
Ion Source Gas 2: 30 mL/min
Run Time: 2 min
Acquisition Mode: MRM
Instrument: Agilent 5975i GC-MS systemGC Parameters: MS Parameters:Column: Restek Stabilwax (30 m × 0.25 mm id × 0.25 µm df) Scan Range: 29-400
with a 5 m retention gap Threshold: 100Inlet Temperature: 250°C Solvent Delay: 4 minTransfer Line Temperature: 250°C MS Temp: 230°C Source Injection: 20:1 Split 150°C QuadrupoleInjection Volume: 1 µL Sampling Rate: 2Carrier Gas: He @ 35 cm/sOven Temperature:
100°C (1 min) to 250°C (4 min) @ 10°C/minTotal Run Time: 20 min
Glycol Composition by GCMS
Litzau J, Mulligan K.“Gas Chromatography - Mass Spectrometry (GC-MS) Screening Procedure for the Presence of Diethylene Glycol and Ethylene Glycol in Toothpaste.” U.S. Food and Drug Administration 2007.
Persian Winter (v:v)PG:VG 47:53
Pro
pyle
ne g
lyco
l
1,4
But
aned
iol
(IS
TD
)
Gly
ceri
n
Headspace GC/FID Analysis Instrument: Tekmar HT3 Headspace sampler (HS)Shimadzu 2014 Gas Chromatograph (GC) with a flame ionization detector (FID)
HS-GC/FID Parameters:Column: Restek RTX-BAC1 (30 m x 0.32 mm id x 1.80 µM)Platen Sample Temp: 80°C Injection: 20:1 Split Sample Equilibrium Time: 3.5 min Detector Temp: 225°C Purge flow: 0.5 mL/min Carrier Gas: He @ 6.75 mL/minInlet Temperature: 200°C Oven Temperature: 50°CTransfer Line Temperature: 160°C Total Run Time: 5 min
E-liquid
- 50:50 PG:G
- 12 mg/mL Nicotine
E-cig voltage: 3.9, 4.3, 4.7
Puff Topography:
– Duration: 4s
– Flow rate: 2.3 L/min
– Interpuff interval: 20s
Allows atomizer to cool
Allows wick to resaturate
Volume in trap:150 mL deionized H2O
E-cigarette tank weighed before and after activation
Aliquot from flask analyzed by HPLC-MS/MS
– 250 ng/mL nicotine-d4 ISTD
Analysis of E-Cigarette Aerosols
KangerTech AeroTank
1.8Ω preassembled atomizer
eGo-V2 variable voltage battery
Analysis of E-Cigarette Aerosols
Water Trap to capture aerosol
– Tygon tubing
– Two 250 mL filter flask in tandem
– Disposable 5mL graduated pipette
– Glass wool plug
– Vacuum pump
– Septum installed in stopper to allowSPME sampling
E-Cigarette
– KangerTech AeroTank, 1.8Ωpreassembled atomizer
– eGo-V2 variable voltage battery
Farsalinos, K. E., G. Romagna, D. Tsiapras, S. Kyrzopoulos and V. Voudris. "Evaluation of Electronic Cigarette Use (Vaping) Topography and Estimation of Liquid Consumption: Implications for Research Protocol Standards Definition and for Public Health Authorities' Regulation." Int J Environ Res Public Health 10, no. 6 (2013): 2500-14.
Goniewicz, M. L., T. Kuma, M. Gawron, J. Knysak and L. Kosmider. "Nicotine Levels in Electronic Cigarettes." Nicotine Tob Res 15, no. 1 (2013): 158-66.
Solid-Phase MicroExtraction
Uses equilibrium to adsorbvolatiles or semi-volatiles inaerosol onto coated fiber surface
Thermal desorption from GCinjection port or DART-MS heliumstream
Coated with Polydimethylsiloxane(PDMS)
– Suitable for non-polarcompounds
– Adsorbs volatiles (MW 60-275)
http://www.sigmaaldrich.com/technical-documents/articles/reporter-us/bioanalysis-with-spme.html
Nicotine E-liquids
27 e-liquids
Labeled nicotine concentrations rangingfrom 6-22 mg/mL
U.S. Products
Vendor Flavor Flavorants FoundBombies White Gummy Bear Benzaldehyde, Methyl anthranilateBryce's Vanilla Cream Custard Vanillin/Methyl salicylate, Ethyl vanillin, Ethyl homovanillateCoval Vapes Mayflower Ethyl vanillinFive Pawns Grandmaster Vanillin/Methyl salicylate, Ethyl vanillin, Ethyl homovanillateGood Life Vapor El Kamino Vanillin/Methyl salicylateGremlin Juice Birthday Cake Vanillin/Methyl salicylate, Ethyl vanillin, Ethyl homovanillateGremlin Juice Kentucky Mint Julip CarvoneGremlin Juice Vanilla Custard Vanillin/Methyl salicylate, Ethyl vanillin, Ethyl homovanillateIndigo Vapor Birthday Cake Vanillin/Methyl salicylate, Ethyl homovanillateMt. Baker GWAR Spew Isoamyl acetateS&S Mods Grumpy's Hooch Vanillin/Methyl salicylate, Ethyl vanillin, Ethyl homovanillateSeduce Juice Jango Vanillin/Methyl salicylateSeduce Juice Pharaoh None identifiedSeduce Juice Snake Eyes Vanillin/Methyl salicylate, Ethyl vanillin, Ethyl homovanillateSeduce Juice Snake Oil Vanillin/Methyl salicylate, Ethyl vanillin, Ethyl homovanillateStLVapor Spearmint CarvoneVapeWell Cheery BenzaldehydeVelvet Cloud Vapor Vanilla Tobacco Vanillin/Methyl salicylate
DART – 8 Flavors Identified in 18 of 27 E-liquids
Nicotine Label vs ActualAmerican Produces
Nicotine 6-22 mg/mL
>10% Diff:
18 of 27
>20% Diff:
9 of 27
>30 % Diff
5 of 27
Range:
-47% to +39%
Measured LabeledE-liquid %PG %G %PG %G258 Rally Squirrel 60 40 - -Captain Ron 45 55 50 50Cheery 33 67 - -Delta 28 72 50 50El Kamino 46 54 - -FennetHIGH 100 0 - -Grandmaster 67 33 50 50Gremlin Juice Birthday Cake 46 54 50 50Grumpy's Hooch 55 45 50 50GWAR Spew 48 52 50 50Indigo Birthday Cake 46 54 50 50Jango 49 51 50 50Kentucky Mint Julip 54 46 50 50Mayflower 22 78 30 70Peach Tobacco 43 57 50 50Pharaoh 61 39 50 50Snake Eyes 47 53 50 50Snake Oil 54 46 50 50Spearmint 51 49 - -Sunset 43 57 50 50Turkish Tobacco 81 19 50 50Unflavored PG 100 0 100 0Vanilla Cream Custard 42 58 - -Vanilla Custard 48 52 50 50Vanilla Tobacco - 100 - 100VG (12 mg/mL) - 100 - 100White Gummy Bear - 100 - 100
Glycol Label vs Actual (%v:%v)6 No description
Labeled Ratio (%v:%v)# (PG:G)
16 50:50
1 30:70
1 100:0
3 0:100
17 were ±10% of the label
Labeled as 50:50 (PG:G) >10%Delta 28:72
Grandmaster 67:33
Pharaoh 61:39
Turkish Tobacco 81:19
0
5
10
15
20
25
Num
ber
of E
-liq
uids
Concentration of Ethanol in % by Weight per Volume
ND = None Detected
Headspace FID Analysis of 63 E-Liquids
SPME GC-MS: StlVapor Spearmint
–Carvone
–Nicotine
SPME fiber injected on Agilent 5973/6890N GC/MS
Thermal desorption: 15 mins
Mass Spec ParametersRamp: 120-300°C, 10°C/min Inj Temp: 275 °C (Splitless)Column: Restek HP-5MS,
0.25mm x 30 m x 250 µm
–Propylene glycol
–Glycerin
Poppy
Morphine – None Detected
Energy Boost, Love, Relax
Herbal Products: E-liquids
Wormwood, Damina, Passionflower
Caruaba Bark, Catnip, Maca Root, Poppy
100 % glycerin
240-3100 mg/mL Ethanol
Will blow your mindLotus Extracts
Apomorphine - psychoactive alkaloiddopamine agonistsParkinson's disease EuphoriaErectile dysfunction VomitingAlzheimer
NuciferineSedationHypothermiaPtosisCatalepsy
Nymphaea caerulea/Blue Lotus
Cotton Wick
Drip Well
Contact Coil
Positive Post
Negative Posts[Atomizer Base – Top View]
E‐liquid“dripped”directlyontothecoiland/orwick
A Tobeco Plume Veil V1.5 Clone dripper
Rebuildable Dripping Atomizer (RDA)
Leaves are harvested for use
Dose dependent psychoactive effects
– Small Doses - Stimulant
– Large Doses - Opioid-like
Kratom
King Kratom(0 mg)
King Kratom (12 mg)
7-Hydroxymitragynine
Mitragynine
8084
93
106
117
120
130
132163 185
226
238
385
399
400
415
0
50
100
Re
l. In
ten
sit
y %
50 200 350 500 650 800
m/z
Pro
plye
ne G
lyco
l
Nic
otin
e
Gly
ceri
n
DART-MS Analysis of King Kratom (0 mg)
7-H
ydro
xym
itrag
ynin
e
Mitr
agyn
ine
Vitamins: E-liquids
Complex flavor arrays
VitaCig® eJuice include: Vitamins A, B, C, E, & CoQ10 (Ubidacenone).
http://www.vitacig.org/vaping-e-liquids/#sthash.
Vitamin E-Liquids: Are they worth it?
–http://www.vitacig.org/discover
–http://dietarysupplementdatabase.usda.nih.gov/ingredient_calculator/help.php#q10
• Vitamin A: 1 IU is the biologicalequivalent of 0.3 mcg retinol, or of 0.6mcg beta-carotene
• Vitamin E: 1 IU is the biologicalequivalent of about 0.67 mg d-alpha-tocopherol, or 0.9 mg of dl-alpha-tocopherol.
• Typical recommended dosages:
• Vitamin A: 5,000 IU
• Vitamin B1: 1.1-1.2 mg
• Vitamin C: 60 mg
• Vitamin E: 30 IU
• CoenzymeQ10: 22-400 mg
Energy: E-liquids
(66:34) PG:G
Ethanol – 140,000 mg/L
Labeled - 0.6 mL/10mL Caffeine Actual 600 mg/mL
Contains: Propylene glycol, Glycerol, Energy Shisha®
Flavouring, Caffeine (0.3% per ml) and Taurine.
http://www.energyshisha.com/
Energy: E-liquids
CBD E-liquids
FDA Issues Warning Letters to CBD Hemp Oil MakersBY SIRIUS J · MON MAR 09, 2015
“Many of these companies claim on their websites that their products are completely legal because they are made from hemp and don’t have any psychoactive properties. The truth is they exist in a legal vacuum as long as they don’t market their products as drugs”
http://www.hightimes.com/
Cannabidiol (CBD)
Pro
pyle
ne G
lyco
l
Veg
etab
le G
lyce
rin
SP
ME
Art
ifac
t
Eth
yl M
alto
lB
enza
ldeh
yde
Pro
pyle
ne G
lyco
l Ace
tal
SP
ME
Art
ifac
t
γ-N
onal
acto
neV
anil
linD
imet
hyl A
nthr
anil
ate
Eth
yl V
anil
lin
Pro
pnyl
guae
thol
6-M
ethy
lcou
mar
in
Hel
iotr
opin
e P
ropy
lene
Gly
col A
ceta
l
Ben
zyl B
enez
enea
ceta
te
Can
nabi
diol
Win
e E
ther
Can
nabi
diol
Pro
pyle
ne G
lyco
l
Veg
etab
le G
lyce
rin
SP
ME
Art
ifac
t
SP
ME
Art
ifac
tIs
omen
thol
Ace
tate
Van
illin
γ-D
ecal
acto
ne
Pea
ch L
acto
ne
Yellow Brick Road
Easy Rider
CBD E-liquids SPME-GC/MS
Easy RiderCompound Formula (MW g/mol) (MW g/mol) DART-MS [M+H]+ SPME-GC/MS RT (min)Propylene Glycol C3H8O2 76.094 77.074 1:27Glycerin C3H8O3 92.093 93.065 1:51Ethyl Maltol C7H8O3 140.137 141.061 3:07Benzaldehyde Propylene Glycol Acetal C10H12O2 164.204 ND 3:45Wine Ether C11H22O2 186.291 ND 3:44y-Nonalactone C9H16O2 156.224 157.123 4:28Vanillin C8H8O3 152.147 153.065 4:50Dimethyl Anthranilate C9H11NO2 165.192 166.091 4.95Ethyl Vanillin C9H10O3 166.174 ND 5:24Propenylguaethol C11H14O2 178.231 179.112 6:056-Methylcoumarin C10H8O2 160.052 161.065 6:34Heliotropine Propylene Glycol Acetal C11H12O4 208.213 209.074 7:14Benzyl Benzeneacetate C15H14O2 226.274 ND 9:06Cannabidiol C21H30O2 314.464 315.232 14:39
Yellow Brick Road Compound Formula (MW g/mol) (MW g/mol) DART-MS [M+H]+ SPME-GC/MS RT (min)Propylene Glycol C3H8O2 76.094 77.074 1:27Glycerin C3H8O3 92.093 93.065 1:51Isomenthol Acetate C12H22O2 198.302 ND 3.82Vanillin C8H8O3 152.147 153.062 4:50Peach Lactone C11H20O2 184.146 185.151 5:29y-Decalactone C10H18O2 170.252 171.141 6:35Cannabidiol C21H30O2 314.464 315.232 14:39ND = Not Dectected By DART-MS
CBD E-liquids DART vs SPME-GC/MS
Cloud 9 E-LiquidLabeled (mg/L)
Actual (mg/L)
Yellow Brick Road 3.3 6.5Easy Rider 3.3 7.6
Concentration of PG:VG, Ethanol & CBD Found in E-liquids
Compound Yellow Brick Road Easy RiderPG:VG (v:v) 35:65 35:65
Ethanol (mg/L) 3600 6600
1973: Oregon decriminalizes cannabis
1927: 1st E-Cigarette patented by Joseph Robinson
2003: 1st Modern E-cig developed in China
2007: E-cigarette use spreads to the U.S.
2006: E-cigarette use spreads to Europe
1996: California legalizes medical cannabis
2012: Washington and Colorado legalize recreational marijuana
2015: Washington DC legalizes recreational MJ
E-cigs and Marijuana
Enhance your experienceDiscreet, Hassle-Free Pleasure
http://jujujoints.com/home
HEALTHNo Smoke, but Haze Around E-Joint
By KIRA PEIKOFF JAN. 12, 2015
http://www.nytimes.com/2015/01/13/health/with-the-e-joint-the-smoke-clears-.html?_r=0
E-liquid Marijuana Formulation
http://mylibertyreach.com/
E-liquid Marijuana Formulation
E-liquid Marijuana Formulation
Labeled Contents
THC – 69.1%
CBD – 1.0 %
Infused with marijuana or active compound of marijuana and food grade propylene glycol
100 150 200 250 300 350 400 450 500 550m/z
%
20
40
60
80
100
315.
2320
359.
2249
311.
2054
317.
2434
331.
2294
–205
.195
7
–77.
0602
Propylene Glycol
137.
2418
Terpene ?
155.
2571
223.
3741
DART-MS Spectra at 20 V of the E-liquid Marijuana Formulation
Tetrahydrocannabinolc (THC) Cannabidiol (CBD) Cannabichromene (CBC)
Cannabinol (CBN)
Cannabigerol (CBG)
Tetrahydrocannabinolic Acid-A (THCA-A)
5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.000
2000
4000
6000
8000
10000
12000
14000
16000
18000
Time (Minutes)
Abundance
Pro
pyle
ne
Gly
col
α-P
inen
e
β-M
yrce
ne
β-P
inen
e
Lim
onen
eL
inal
ool
Fen
chyl
Alc
ohol
Bor
neol
Terp
ineo
l Β-C
aryo
phyl
lene
α-H
umul
ene
Gua
iol
Ced
rol
α-B
isab
olol
GC/MS Identification of Propylene Glycol and Terpenes
HPLC-MS/MS Identification of Cannabinoids
J.L. Poklis et aL. J. Anal. Toxicol. 2010, 8. 516-520.
Compound Advertised Conc
(%) Actual Conc
(%) Tetrahydrocannabinol (THC) 69.1 42.6Cannabidiol (CBD) 1.0 0.5Cannabinol (CBN) NA 0.36Cannabichromene (CBC) NA 0.72Cannabigerol (CBG) NA 0.64Tetrahydrocannabinolic Acid-A (THCA-A) NA 5.6NA = Not Advertised
Concentration of CannabinoidsFound in E-liquid
Shanks K.G. Detection of Synthetic Cannabinoids in Two E-Cigarette Liquids, SOFT October,20 2015
Buzz Juice Liquid Incense (Unflavored)
MAB-Chminaca 2.1 mg/mL
AB-Chminaca 23 µg/mL
AB-Pinaca 4.6 µg/mL
ADB-Pinaca 164 ng/mL
Buzz Relax E-Juice(Maple Syrup/Rum flavored)
XLR11 6.0 ng/mL
AB-Pinaca <0.2 ng/mL
5F-PB-22 <0.2 ng/mL
PB-22 <0.2 ng/mL
E-liquid & Designer Drugs
Identify E-liquids
The container
Contains propylene glycol and/or glycerin
Smell - flavoring components
Dried resins or powders
Go to the website
This project was supported by:
U.S. Department of JusticeAward No. 2014-R2-CX-K010
National Institutes of Health Grant No. P30DA033934
The opinions, findings, and conclusions or recommendations expressed in this presentation are those of the author and do not necessarily reflect those of the Department of Justice.
Funding NIHNational Institutes of Health
Acknowledgements E-Cigarette Research Group
Virginia Commonwealth University Dr. Michelle R. Peace Dr. Alphonse Poklis Dr. Carl E. Wolf Haley A . Mulder Rose I. Krakowiak Tyson R. Baird Karen E. Butler Shelly Butler Joseph W. Stone
Questions?
Justin R. Victoria, B.A. Ocean County Sheriff’s Office
144 CHESTNUT STREET • TOMS RIVER, NEW JERSEY 08753 PHONE (732) 288-7615
Justin Victoria received his Bachelor of Arts degree in Chemistry from
Gettysburg College in 2013. He is completing his third year as a Forensic
Chemist for the Ocean County Sheriff’s Department. As a Forensic Chemist,
Justin has worked primarily in the area of drug analysis. In addition to his
everyday case work, Justin has been involved with studying electronic cigarette
usage for the consumption of illicit materials.
E-CIGARETTE CASES
OCEAN COUNTY SHERIFF’S OFFICE FORENSIC SCIENCE LABORATORY
-JUSTIN R. VICTORIA
FORENSIC CHEMIST
-MATTHEW R. WOOD
LABORATORY DIRECTOR
DISCLOSUREThe authors have no financial or other relationship with the manufacturer of any commercial products or providers of any commercial service or supporters. No product or instrument manufacturers listed or discussed within this presentation provided any financial support for this project.
The views expressed are of the author(s) alone and do not reflect the policies, procedures, or opinions of the Ocean County Sheriff’s Office.
The opinions, findings, and conclusions or recommendations expressed in this workshop are those of the author(s) and do not necessarily reflect those of the Department of Justice.
NEW JERSEY PUBLICLABORATORIES
NJSP North Regional Lab Little Falls, NJ
NJSP East Regional Lab Sea Girt, NJ
NJSP Technology Complex Hamilton, NJ
NJSP South Regional Lab Hammonton, NJ
Ocean County Sheriff’s Office
Forensic Science Laboratory
SUMMARY• Eight (8) cases analyzed from 2013-2015
• One (1) e-cigarette positive for nicotine.• Four (4) vaporizers/vape-pens positive for
THC.• One (1) e-liquids positive for nicotine.• One (1) e-liquid negative for both THC and
nicotine.• One (1) e-liquid positive for THC.
• All samples tested via GC-MS
• “General Screen” Method ~20mins• 65ºC-2min; 20ºC/min ramp; 300ºC-6min• 30m x 0.25mm, 0.1µm –
5% diphenyl dimethyl polysiloxane• Electron Ionization (EI), positive mode
0742-13Submitted 2/22/13 from OCPO
NJOY brand e-cigarettes
• One (1) E-cigarette and box
• Also Submitted
• Bag with pills
(quetiapine)
0742-13RESULTS
0854-14Submitted 2/20/14 from Ocean Twp.
One vape pen with glass bulb
• Vape pen of unknown brand
• Also submitted• Three (3) non-electronic
smoking devices
• One (1) grinder
• Three (3) sources of THC(hashish, burnt vegetativeresidue)
0854-14RESULTS (BULB)
1812-15Submitted 6/3/15 from Seaside Heights
TOKN brand vaporizer
• One (1) Vaporizer
• Also Submitted• vegetation
1812-15RESULTS
2031-15Submitted 6/17/15 from Lakewood
Drug overdose (No charges filed - immunity)
One (1) bottle of Vapors E-Liquid• Also submitted
• Syringe• Used wax folds
2031-15LABEL
Front Label: VAPORS Original E-LiquidManufactured for Vapors, Brick, NJ 08723www.vaporstoreonline.com
Back Label: WARNINGThis product intended for use or purchase by persons 18 years or older. Do not drink. Do not spill on your skin. Keep out of reach of children and pets.INGREDIENTSMAY OR MAY NOT CONTAIN:USP Grade Propylene Glycol, USP Grade Vegetable Glycerin, Deionized Water, Natural Flavors, Artificial Flavors, USP Grade NicotineSHAKE WELL
Slight odor of cherry tobacco. Website: ~36 flavors $5.99-6.99 0 – 24mg nicotine
2031-15RESULTS
SUBSTRATE & POSITIVE CONTROLS
2263-15
Submitted 7/6/15 from Ocean Twp.
One vape pen
• Juvenile
• One (1) Vape pen of unknown brand
2263-15RESULTS
3652-15
Submitted 10/1/15 from Ocean Twp.
One (1) Seego VHit Reload vaporizer
• Vegetation visibleinside device
• Also submitted• Vegetation
3652-15RESULTS
*Case # since amended
3664-15
Submitted 10/1/15 from Jackson
One (1) oral syringe with brown liquid
• Also Submitted• Large quantity
of vegetation
• Three (3) bagsof vegetation
3664-15RESULTS
SPE SAMPLE PREP1. 1mL e-Liquid + 1mL Methanol + 4mL 100mM Phosphate Buffer pH 6.0
(vortexed)
2. UCT Clean Screen® CSTHC203 Extraction Column
3. Condition Column
1. 3mL Methanol2. 3mL Water3. 1mL 100mM Phosphate Buffer pH 6.0
4. Load Sample
5. Wash Column
1. 3mL Water2. 3mL 100mM Phosphate Buffer pH 6.0
6. Dry Column
7. Elute THC
1. 3mL Hexane/Ethyl Acetate/ Acetic Acid (49:49:2)2. Dry under nitrogen, reconstitute w/ 100uL ethyl acetate
Sample prep modified from UCT Methods, Bristol, PA (Aug 2013)
I6
3664-15RESULTS FOLLOWING SPE EXTRACTION
3664-15RESULTS FOLLOWING SPE EXTRACTION
10.65 – Tetrahydrocannabivarin11.01 – Cannabadiol11.09 – Cannabichrome11.18 – Cannabicoumaronone11.24 – ∆8-THC11.42 – ∆9-THC11.72 – Cannabinol
ACKNOWLEDGEMENTS
Michelle Peace, Ph.D. - Virginia Commonwealth University
Fellow Workshop Presenters
Workshop Attendees
Sergeant James Capaccio – Ocean Twp. PD
Ocean County Sheriff’s Office
• Matthew Wood – Lab Director and Co-author
• Heather Dover – Senior Forensic Chemist
THANK YOU!The preceding case samples only indicate a small sample of the samples and results we see at the lab.
We will continue to monitor the misuse and abuse of e-cigarettes and other related paraphernalia within Ocean County.
Captain Juan Colon New Jersey State Police
Bureau Chief Regional Operations Intelligence Center
Captain Juan Colon is a 23 1/2 year veteran of the New Jersey State Police. Most of his career has focused on the intelligence function, and he has extensive experience with street gangs and organized crime. As an intelligence collector targeting these groups, he has managed numerous informants and has conducted several undercover operations.
He served as the chair of the Information Sharing Environment subcommittee for Super Bowl 48. In this role, he developed the concept of operations which has been used in subsequent Super Bowls and similar large scale events.
He also developed a training program which enabled New Jersey to lead the nation in providing training to private sector security personnel in properly identifying and reporting suspicious activity to help protect critical infrastructure.
He developed and implemented New Jersey’s Fusion Liaison Officer initiative, which includes more than 1100 members of law enforcement, and the private and public sectors.
He developed a process to facilitate information sharing with the El Paso Intelligence Center to ensure that all drug-related information is shared in real time at a national level. This concept is in the process of being implemented for other states to follow.
As result of these efforts, he has received several awards and was nominated for Trooper of the year in 2014.
He is currently assigned as the Bureau Chief of the Information and Intelligence Support Bureau, at the Regional Operations Intelligence Center. He oversees three Units: Intelligence Watch and Warning Unit, Real Time Crime Center North Unit, and Real Time Crime Center South Unit.
His undergrad in degree is in public administration from Fairleigh Dickerson University. As the architect of the Drug Monitoring Initiative, he is involved in several state working groups developed by the Attorney General’s Office to drive State level counter-drug initiatives.
Drug Monitoring InitiativeRegional
An Intelligence Capability for Public Health& Public Safety Partners
FINANCIAL DISCLOSURE
I have no relevant financial affiliations to disclose and no actual or potential conflicts of interest in regard to this presentation.
An Intelligence Capability for Public Health & Public Safety Partners
Intelligence‐Led
Policing
& Prevention
You Can't Manage What You Don't Measure
Enforcement
Prevention
Understand the scope of the drug problem
The presence & prevalence of specific drugs
Enhance policies and practices
BUILDING OUR DRUG INTELLIGENCE CAPABILITY
1. Identify Information Requirements:Investigative ‐ local, county, state, and Federal LE partnersPublic health professionals – treatment and prevention
What information do you need to help you fulfill your job responsibility? What information would make your efforts more effective and impactful?How often do you require updates of the information?What’s missing among our collective anti‐drug efforts?Do you have any recommendations?
2. Identify Essential Data Sets – Derived from requirementsCrimes ‐ Drug Seizures, Shootings, Gun Recoveries, Drug ArrestsHealth ‐ Overdoses, Toxicology Data, Addiction Treatment Admissions
3. Identify Data Sources ‐ DMI met with executives of the entities that gatheressential data sets for investigative or administrative purposes. These data elements would fulfill customers’ requirements.
BUILDING OUR DRUG INTELLIGENCE CAPABILITY
4. Minimize Points of Collection ‐ DMI leverages nodes or centralrepositories as collection points. (Labs, Department of Health, Etc.)
5. Establish Relationships with Source Entities ‐ DMI establishedcollaborative relationships with the executives of the centralrepositories identified.
6. Automate the Information Collection processesDMI relies on real time information, requesting partners to submittheir data daily, and at times, contemporaneous to drug‐relatedincidents such as suspected drug overdoses.
NOTES
NOTES
LtLT
INTELLIGENCE-LED POLICINGINTELLIGENCE-LED OUTREACH
PreventionPreventionEnforcementEnforcement
TreatmentTreatment
Intelligence
• Access
ProcessProcess
• Data
PlatformsPlatforms
• Information
PeoplePeople
Sgt. Adam PolhemusNJ ROIC/[email protected]‐414‐3356
An Intelligence Capability to Understand New Jersey’s Drug Environment
Drug Monitoring Initiative (DMI) OverviewHeroin and opiate use in New Jersey has increased exponentially in recent years. The high rate ofaddiction drives the increased demand for both heroin and prescription painkillers, and recent statisticsidentify an increase in illicit heroin and opiate use, seizures, and deaths. During 2013, the State MedicalExaminer’s Office recorded 1,336 fatal drug overdoses. This common scenario has indiscriminatelyplayed out in New Jersey and across the country, affecting all races, genders, age groups, and socialclasses.
The New Jersey State Police developed DMI in response to this situation and to understand the scope ofthe problem through continuous monitoring of drug activity statewide. The DMI intelligence capabilityestablishes a drug information sharing environment that enables law enforcement, human services, andpublic health experts to better understand trends, patterns, implications, and threats from illicit drugactivity having an impact on specific locations statewide. DMI gathers investigative and administrativedata, both on the supply side and the demand side, to develop a 360 degree view of the State’s drugenvironment. The analysis is used to produce intelligence products for partners across state and localagencies and non profit organizations. This process enables intelligence led policing and investigativesupport for law enforcement and intelligence led outreach for treatment and prevention efforts.
Collection ProcessVarious agencies collect drug data needed to interpret New Jersey’s illicit drug environment. DMIleverages the existing people, processes, and platforms through an information sharing network whichdirects essential drug data sets to DMI for storage, analysis, production, and sharing. DMI leverages thefollowing entities, which provide the respective data elements through data sharing agreements and ina de identified fashion, where appropriate:
State Police and county forensic laboratories – all analyzed drug data
NJ Department of Health (DOH) – EMS Narcan deployments
County Prosecutor’s Offices – Narcan deployments by law enforcement
State Medical Examiner’s Office – Drug involved death data
NJ Mental Health and Addiction Services – Patient admissions and drug use data
Automated Fingerprint Information System – Daily drug arrest data
Prescription Drug Monitoring Program – Collected transactional data
ProductionAll of the information allowed to be shared is normalized and uploaded to the Project SafeNeighborhood Mapping Program, where it is stored, geo coded, mapped, and made available to lawenforcement, human services, and health partners via MAGLOCLEN’s RissNet portal. DMI analysts usethis information to provide:1) Investigative support for strict liability cases and other drug investigations.2) Situational awareness through the following products:
Daily Drug Environment Report – Heroin stamps seized and involved in overdoses are includedin this report along with opiate pills seized in NJ.
Ad hoc Alerts – The NJ ROIC provides heroin overdose alerts, new and emerging drugnotifications, and drug environment products from New Jersey and other regional DMI partners.
Training and OutreachTo increase drug awareness and information sharing, DMI developed the:1) Monthly Conference Call – Brings together law enforcement, health partners, fusion centers andother entities to share information pertaining to drug trends in different areas of the country.
2) Basic Drug Recognition Course – Law enforcement, fire service, EMS, and health partners learn aboutdrugs, trends, identifiers, and how to collect and share drug related information.
DMI Established Best Practices
• Facilitates collaboration among diverse multidisciplinary entities to address the drug problem
• Uses automated drug data collection processes to ensure a timely exchange of information
• Desensitizes information to ensure seamless and transparent information sharing
• Derives intelligence from all investigative and administrative drug data
• Incorporates subject matter experts from various disciplines into the drug intelligenceproduction process
• Supports narcotic investigations and overdose strict liability cases
• Employs the Journey to Drugs methodology to understand a drug’s impact on local areas
• Coordinates collection, analysis, and mapping of drug incident data statewide
• Facilitates expedited analysis of drugs seized through forensic labs
• Uses empirical data as opposed to survey data to understand the drug environment
• Provides drug training for law enforcement, fire service, and EMS personnel
• Provides drug situational awareness for all constituents
• Tracks Naloxone administrations by law enforcement and EMS statewide to identify potentialspikes in drug overdoses
• Provides real time alerts to the public, law enforcement, and healthcare partners of spikes indrug overdoses occurring in specific areas
• Creates & leverages a network of existing people, platforms, and processes
For more information on the Drug Monitoring Initiative, contact Sgt. Adam Polhemusat [email protected] or call 609-414-3356.
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Situational Awareness:
Liquid Marijuana
3 October 2014
(U//FOUO) NJ ROIC Fusion Liaison & Intelligence Training Unit~ROIC201409-03377F
OVERVIEW (U//FOUO) Liquid marijuana is increasingly being identified in New Jersey, and has been attributed to numerous overdoses throughout the country. While medical marijuana has medicinal uses, variations with very high levels of tetrahydrocannabinol (THC) can have dangerous mental and physical health effects. Liquid marijuana is difficult to detect in stores where it is being sold, and while being consumed by users, who are also exploiting electronic cigarettes to consume illegal substances.
POTENCY OF LIQUID MARIJUANA (U//FOUO) Concentrated marijuana liquid is produced from cannabis plant extracts; analysis has revealed THC levels can reach approximately 90%. These levels are much higher than the 10% to 20% THC levels found in common marijuana vegetation. The higher potency poses a risk to users as they may be unaware of the significantly higher levels of THC contained in liquid marijuana or how their bodies will react to its potency. Liquid marijuana is most commonly consumed through the use of electronic cigarettes, which vaporize the liquid. Because the liquid marijuana market is relatively new, it is unknown what long-term side effects will develop as users consume elevated levels of THC.
LIQUID MARIJUANA IN NEW JERSEY (U//FOUO) In May 2014, the New Jersey Division of Consumer Affairs Enforcement Bureau conducted a covert investigation of the Atlantic City Counterculture Exposition where vendors displayed smoking devices and products which were to be sold on the boardwalk during the summer of 2014. During the EXPO, agents purchased an e-liquid product labeled “Holy Grail” for intelligence gathering purposes. The vendor stated that the item did not contain any illegal drugs, but could produce the same effect as marijuana. Laboratory testing later revealed the product contained liquid marijuana.
(U//FOUO) Some small businesses in New Jersey are knowingly selling liquid marijuana products and marketing them alongside other (legal) e-liquids. In Wildwood, NJ, a police investigation was initiated when authorities learned of a boardwalk vendor selling liquid marijuana alongside other e-liquid products. During the
“VAPE PENS”
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PAGE 2 OF 4
investigation, the vendor directed the agents to the liquid marijuana after the agents asked for something that would give them a “high.” Analysis of the seized product revealed that it contained liquid Cannabidiol (CBD), a compound found in marijuana plants. Medical practitioners are increasingly using strains of marijuana with high levels of CBD because it offers the same medicinal values without the psychoactive traits associated with THC.1 CBD is an active ingredient used to treat chronic pain, lupus, Crohn’s disease, and epilepsy since cannabidiol receptors do not shut off breathing or respiration, as other drugs do; long-term effects are still unknown. In New Jersey, CBD is a Schedule I CDS and is currently illegal. Medical patients who fall under the Compassionate Use of Medical Marijuana Act (CUMMA) are authorized to possess, use, and transport the drug.
(U//FOUO) In addition to liquid marijuana, which contains THC and CBD, users are also consuming “synthetic” marijuana, which is a chemically manufactured product designed to mimic the effects of marijuana. It has caused several overdoses and several states have prohibited the sale of these products. In addition to causing subjects to overdose, other health risks include psychosis, epileptic seizures, and heart attacks. Synthetic marijuana products such as “Cloud 9,” “Spice,” and “K2” (pictured right) have been seized in New Jersey. Synthetic marijuana is sold either as a liquid or as vegetation that has been sprayed with synthetic liquid marijuana. These products were routinely marketed as incense and labeled “not for human consumption.”
DETECTION OF LIQUID MARIJUANA (U//FOUO) The combination of liquid marijuana and water vapor in commercial e-cigarettes can mask the odor of marijuana when smoked and may help avoid detection by law enforcement personnel. However, police report that drug sniffing dogs have been able to detect the presence of liquid marijuana in e-cigarettes.
(U//FOUO) Law enforcement officers should also be aware that users may possess syringes, which are used to load the liquid into electronic cigarettes.
HEALTH RISKS OF LIQUID MARIJUANA (U/FOUO) Use of electronic cigarettes and the variety of e-liquid flavors available is appealing to young smokers who are experimenting with new products in the e-cigarette market.2 Continuous use of high levels of THC can lead to long-term health risks, such as breathing problems, cognitive impairment, psychosis, and even
1 Giddingson, J. (2013, 11 20). Chicago Now. Retrieved 09 26, 2014, from www.chicagonow.com: http://www.chicagonow.com/chicago-medical-marijuana/2013/11/cannabidiol-the-side-of-marijuana-you-dont-know/2 Raloff, J. (2014, June 28). Health Risks of E-Cigarettes Emerge. Retrieved September 25, 2014, from http://www.sciencenews.org: https://www.sciencenews.org/article/health-risks-e-cigarettes-emerge
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PAGE 3 OF 4
learning disabilities in children.3 Effects can include agitation, paranoia, hallucinations, chest pains, increased pulse, high blood pressure and suicidal thinking and behavior.4 Liquid marijuana use may cause mental and emotional side effects, and users may experience and exhibit feelings of euphoria, short-term memory loss, difficulty in completing complex tasks, changes in the perception of time and space, sleepiness, anxiety, confusion, and inability to concentrate. Physical side effects may include low blood pressure, fast heartbeat, dizziness, slow reaction time, and heart palpitations. As the e-liquid market is relatively new and unregulated, these products will continue to pose elevated risks as consumers are likely be unaware of the ingredients contained in the e-liquid products they consume.
CONCLUSION (U//FOUO) The decriminalizing of marijuana at the state level, as in Washington and Colorado, has created a legitimate market for liquid marijuana products. As these products are now being legally manufactured and sold in both states, an illicit market for these products has developed enabling drug users to obtain those marijuana variants in other states where the products are not legal. Marijuana liquids are increasingly being seized throughout New Jersey, illustrating the increased supply and growing demand for these products. As variant types of marijuana become more prevalent in New Jersey, law enforcement officers will need to be aware of the variety of products available to users. Due to the concentrated levels of THC, law enforcement personnel should request EMS assistance when they believe they are dealing with an individual who may be experiencing an overdose from liquid marijuana.
(U//FOUO) Merchants’ concealment methods and the growing supply and demand for liquid marijuana and associated products mandate law enforcement and public health officials to proactively identify these products’s presence to reduce health risks and increase public safety.
REFFERAL (U/FOUO) The NJ Governor’s Council on Alcoholism and Drug Abuse (GCADA) has launched a statewide awareness campaign, “Addiction Does Not Discriminate” to help fight drug abuse by showing that no one is immune to the deadly drug problem. This program provides New Jersey residents with information on preventing abuse, recognizing those at risk, and finding treatment. Please go to KnowAddiction.nj.gov to learn more.
REQUEST FOR INFORMATION (U//FOUO) The NJ ROIC Fusion Liaison & Intelligence Training Unit is seeking additional information to assess impact and implications for NJ concerning this topic, in furtherance of the Drug Monitoring Initiative (DMI). Any recipient with further information is requested to contact the NJ ROIC Fusion Liaison & Intelligence Training Unit at [email protected], by fax to 609-530-4174 or by calling 609-963-6900 ext. 6273 or 2044.
3 Brown University Health Services. (2014, 08 15). Brown University . Retrieved 09 24, 2014, from http://www.brown.edu/Student_Services/Health_Services/Health_Education/alcohol,_tobacco,_&_other_drugs/marijuana.php
4 Paul, M. (2013, December 16). Northwestern University Newscenter - Research. Retrieved September 25, 2014, from www.Northwestern.edu: http://www.northwestern.edu/newscenter/stories/2013/12/marijuana-users-have-abnormal-brain-structure--poor-memory.html#sthash.52diCQLP.dpuf
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PAGE 4 OF 4
(U//FOUO) Through the DMI, the State Police Regional Crime Labs will facilitate expedited forensic analysis to assist investigators and health care professionals during emergent situations. Any law enforcement agency requiring expedited analysis of suspected drug specimens involved in overdoses should contact the NJ ROIC Fusion Liaison & Intelligence Training Unit at [email protected], by fax to 609-530-4174 or by calling 609-963-6900 ext. 6273 or 2044.
(U//FOUO) The Compassionate Use of Medical Marijuana Act (CUMMA) was signed into law to protect from arrest, prosecution, property forfeiture, criminal and other penalties, those patients who use marijuana to alleviate suffering from debilitating medical conditions, as well as their physicians, primary caregivers, and those who are authorized to produce marijuana for medical purposes. The Department of Health has promulgated regulations for the implementation of the Act and serves as the lead state agency in developing the Medicinal Marijuana Program (MMP) in the state of New Jersey.
(U//FOUO) The Office of Attorney General developed Enforcement Guidelines to provide Law Enforcement with guidance and instruction on key provisions of the Act. This document is available at the Division of Criminal Justice website under AttorneyGeneral Guidelines (http://www.njdcj.org/agguide.htm). The MMP, in cooperation with the Department of Law and Public Safety, has established an MMP Identification Card validation process. Law Enforcement personnel that encounter or have questions regarding the validity of an MMP Identification Card should contact the New Jersey State Police, Regional Operations Intelligence Center (ROIC) for Identification Card validation.
(U//FOUO) The MMP has three (3) permitted and operational Alternative Treatment Centers: 1) Greenleaf Compassion Center in Montclair, 2) Garden State Dispensary in Woodbridge, 3) Compassionate Care Foundation in Egg Harbor. These facilities dispensemedicinal marijuana in raw vegetative form and are in the process of developing protocols for the manufacturing of lozenge, topical formulations and edible products. As these products become available, Law Enforcement will be notified and provided with appropriate instruction on identification. Additional information regarding the Medicinal Marijuana Program is available at http://nj.gov/health/medicalmarijuana/index.shtml.
