Profiling of Illicit Diazepam Tablets for

Drug Intelligence Purposes –

A Case Study

R-LINCS

Valium is killing Scotland’s Drug taking Poor

William Nicoll, Photos: Harrison Reid  Mar 14 2013

“Jack explains that there's an anagram hidden in the word methadone: "the mad one". We both laugh. Then we search for anagrams in the word Valium, but there are none. After methadone, Valium is the drug that is killing Scotland, contributing to, or responsible for 32% of drug-related deaths in 2011”.

Diazepam is killing Scotland’s Drug-Taking Poor

William Nicoll, Photos: Harrison Reid  Mar 14 2013

When Valium – or diazepam, as it's technically called in Scotland – turned 40, drugs manufacturer Hoffmann La Roche held a celebration where they unfurled a banner that read: "Thanks for the happiness and relaxation you have given us over the years.“

Thanks to “Mother’s Little Helper" and the majority of late 20th century American fiction, many of us have been left with the mistaken belief that Valium is the preserve of the clinically bored, middle-aged housewife, when really the drug is killing Scotland's poorest men – detected in the bodies of 72% of all victims of drug-related death.    Jack can attest to Valium’s power; he's been addicted to the drug for 19 years and had taken 28 pills before meeting me. While he concedes that they were "whites" (the lower strength two milligram tablets, as opposed to the stronger "blues"), that amount is still more than nine times the effective daily dose for anxiety.

Background• Started with diazepam analysis for student

projects in 2012• Police Scotland – Kenny Simpson• Discussions with Isobel Stewart• Required to get Crown Office permission to use

tablets from closed cases• It was thought that this work could be expanded

to provide drug intelligence information• Awarded R-LINCS (Research-Led Innovative Nodes

for Contemporary Society) PhD studentship from Abertay

• Began collaboration on the project with Police Scotland and RGU in September 2013

BackgroundAims of the R-LINCS Project: To provide drug intelligence information that could assist the police in determining links between different seizures. This will be attempted through the measurement of certain physical and chemical characteristics of illicit tablets and the extraction of information from the data set to construct a statistical model to identify different populations.

Scoping exercise Photography Tablet Weight and Measurements Diazepam quantification through HPLC (+RGU) DSC (RGU) Thermal Gravimetric Analysis (RGU) Scanning Electron Microscopy (RGU) GC-MS for the identification of active drug substances

(+RGU) Energy Dispersive X-Ray Analysis (RGU) Adulterants (+RGU) Identification of colourants Quantification of sugar – lactose?? Tabletting (RGU)

Initial selected Parameters

Photography

Tablet Weight and Measurements

Diazepam quantification through HPLC

GC-MS for the identification of active drug

substances

[Analysis of Dyes through UV-Vis]

[Analysis of Sugars through HPLC]

Photography

Images recorded using an Olympus DSX100 microscope on loan from Olympus

Diazepam Analysis

Analytical Results of All Cases Received (54)• 67% Diazepam Drug Substance

• 33% “Other” Drug Substances

Analytical Results of Cases from 2013 (11)• 27% Diazepam Drug Substance

• 73% Other Drug Substances

Diazepam Quantification from All Cases Received• Only 32% contain 10mg of Diazepam

• Highest recorded diazepam content = 48mg

From a total of 1715 tablets analysed:

DiazepamFirst marketed as Valium by 

Hoffmann-La-Roche is the archetypical

benzodiazepine drug used to treat anxiety, panic attacks insomnia

and seizures 

PhenazepamNo methyl on

Nitrogen and a bromine in place of the chlorine

and extra chlorine in the non-fused

phenyl ring.

EtizolamBenzene ring has been replaced by a thiophene ring, making the drug

a thienodiazepine.It is also a fused

triazole

Benzodiazepines

Plus other non-benzodiazepines

The Database

Tablet Weights

Imprint Details

Identification and Quantification of Main Drug

Substance

Identification of Dyes

Identification of Main Excipients

Used to Build A Statistical Model

The Database

The database requires constant updating as further results are

produced.

This will create an easily accessible tool for comparison and

analysis of data.

In addition, the use of statistical techniques should help with the

visual interpretation and understanding of the results.

At present the statistical analysis on the weight of the tablets has

been utilised

Early work using ‘Miner 3D’ produces an interesting and useful way

to visualise the results.

Grouping of tablets using Miner 3D

Illicitly manufactured tablets having 10 mg

Do not contain diazepam

Contain greater than 20 mg diazepam

Possibly pharmaceutical grade

Diazepam content

Std. Dev of Weight

Ave. of Weight

Results so far

Genuine tablets (red) and Probably genuine

Counterfeit tablets

Variability in Level of Diazepam

Different Active Drug Substances

Potential Diverted Pharmaceutical Tablets

Tablet Mass

The Future

Dyes

Sugars

More Statistical

modelling

The Further Future

ECSTACY

The Collaboration• Kenny Simpson (Police Scotland)

• David Bremner (AU)

• Kevin Farrugia (AU)

• Mae MacDougall-Heasman (AU)

• Anne Savage (AU)

• Isobel Stewart (AU)

• Graham Wightman (AU)

• Kerr Matthews (RGU)

• Raymond Reid (RGU)

• Ann Tough (RGU)

• Stuart Waddell (RGU)