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SAMPLE
Matrix: blood
Sample preparat ion:
Condition a Bond-Elut C18 SPE cartridge with M eOH and water.
Add
500 |xL
plasma
to the SPE
cartridge, wash with
2 mL
water, wa sh with
2 mL
MeO H: water 20:80 , elute w ith
two 500
|JLL aliquots
of
MeOH. Evaporate
the
eluate
to
dryness under a stream of nitrogen, reconstitute the residue in 50 |xL MeOH : water 20:
80,
inject a 20 JULL aliquot.
HPLCVARIABLES
Column:
100 X 1 5 |xm Hyp ersil ODS
Mobile phase:
MeCN : MeO H: water 25:25 :50
Flow rate: 0.1
Inject ion vo lum e:
20
Detector: UV
CHROMATOGRAM
Retent ion t ime:
20
Limit of detect ion:
2
ng/mL
OTHER SUBSTANCES
Extracted:
androstenedione, 20a-hydroxy-4-pregnen-3-one, 17a-hydroxyprogesterone, pro-
gesterone, testosterone
KEYWORDS
microbore; rat; plasma; SPE
REFERENCE
Taylor,
R.B.;
Kendle,
K.E.;
Reid,
R.G.;
Hung,
CT.
Chromatography
of
progesterone
and its
major
me-
tabolites
in rat
plasma using microbore high-performance liquid chromatography columns with
con-
ventional injection
and
detection systems. J.Chromatogr.,
1987, 385,
383—392
SAMPLE
Matrix:
blood
Sample preparat ion:
2 mL
Plasma
5 mL
hexan e: dichloromethane
1:1,
shake
for 10 min,
centrifuge at 2000 rpm for 10 min. Remove 4 mL of the organic phas e and evaporate it at
55° under nitrogen. Reconstitute residue in 300 |xL mobile p has e, inject a 150 |xL aliquot.
HPLCVARIABLES
Column:
250 X 4.6 5 |xm
L iChrosorb
RP-8
Mobile phase:
MeO H: MeCN : water 20:30 :50
Flow rate: 2
Inject ion volume:
150
Detector:
UV 254
CHROMATOGRAM
Retent ion t ime: 8
Limit
of
qu ant i ta t ion:
2
ng/mL
Norethindrone
Molecular formu la: G
20
H
26
O
2
Molecular weight:
298.4
CAS Registry No :
68-22 -4, 51-98-9 acetate)
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KEYWORDS
plasma
REFERENCE
Loo,
J.C.K.;
Brien,
R.
Analysis
of
norethindrone
in
plasma
by
high-performance liquid chromatography.
J.Liq.Chromatogr. 1981
4
871-877
SAMPLE
Matrix: bulk
HPLCVARIABLES
Column:
250 X 4 10 jxin LiChrosorb RP-18
Mobile phase: MeOH: water 70:30
Flow rate: 1
Injection volume: 25
Detector: UV 240
CHROMATOGRAM
Retent ion t ime: 7
OTHER SUBSTANCES
Simultaneous:
ethinyl estradiol, impurities, norgestrel
REFERENCE
Gdrdg, S.; Herenyi, B. Analysis of stero ids . XXXVIIL The use of high-performance liquid chrom atography
with diode-array
UV
detection
for
estimating impurity profiles
of
steroid d rugs. J.Chromatogr.
1987
400
177-186
SAMPLE
Matrix: food
Sample preparation:
Dissolve apple extracts in THF, inject a 10 |xL extract.
HPLCVARIABLES
Column:
300 X 3.9 jxBondapak C18
Mobile phase: MeOH: THF: water 11:26:63
Flow rate: 1.7
Injection volume: 10
Detector: UV
254
CHROMATOGRAM
Retention time: 11.6
OTHER SUBSTANCES
Simultaneous:
degradation products, impurities
KEYWORDS
apples; fruit; stability-indicating
REFERENCE
Mayberry, D.O.; Kow blansky, M.; L ane, RA.; Wray, RE. Determination of norethindrone stability on Red
Delicious apples. J.Pharm.ScL
1990
79 746-749
SAMPLE
Matrix: formulations
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Sample p re par at io n : Dissolve 12 tablets in 600 mL water with stirring at 75 rpm, remove
3 mL sample, centrifuge at 3000 rpm for 15 min, inject a 250 |xL aliquot.
HPLCVARIABLES
Colu mn: 100 X 4.6 3 jxm Phenomenex IB-SiI 3 C18
Mobile p ha se : MeCN: water 40:60, pH 5.6
Flow rate: 1.2
Injection volume: 250
D etec tor: UV 200
C H R O M A T O G R A M
Retention time: 7.7
OTHER SUBSTANCES
Simultaneous: ethinyl estradiol
KEYWORDS
tablets; modification of USP method
REFERENCE
Dorantes, A.; Stavchansky, S. Modification of the U.S.P. dissolution method for the analysis of noreth-
indrone and ethinyl estradiol tablets. J.Pharm.ScL 1994, 83 3 7 9 - 3 8 1
SAMPLE
Matrix: formulations
Sam ple p re pa ra tion : Dissolve 6 tablets in 600 mL water: isopropanol 97:3, remove 5 mL
samples, centrifuge at 1500 rpm for 10 min, inject a 50-200 |xL aliquot.
HPLCVARIABLES
Column: 300 X 3.9 10 jxm Bondapak C18
M obile ph as e: MeCN: water 55:45
Flow rate: 1
Injection volume: 50-200
Detec tor: UV 200
OTHER SUBSTANCES
Simultaneous: mestranol
KEYWORDS
tablets; modified USP method
REFERENCE
Nguyen, H.T.; Shiu, G.K.; Worsley, W.N.; Skelly, J.R Dissolution testing of norethindrone: ethinyl estra-
diol, n orethindrone : mestranol, and norethindrone ace tate: ethinyl estradiol combination tablets.
J.Pharm.ScL 1990 79 163-167
SAMPLE
Matrix: formulations
Sa m ple p re para ti on : Dissolve 6 tablets in 600 mL 100 mM HCl containing 0.02 sodium
lauryl sulfate, remove 5 mL samples, centrifuge at 1500 rpm for 10 min, inject a 50-200
IxL aliquot.
HPLCVARIABLES
Colu mn: 220 X 4.6 5 |jim Spheri-5 C18
Mobile p has e: MeCN: 20 mM pH 6.0 phosphate buffer 35:65
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Inject ion vo lum e:
10
Detector:
U V 240
CHROMATOGRAM
Retent ion t ime:
4.6 (norethindrone), 8.6 (norethindrone acetone)
Limit of detect ion: 5 jig/mL
OTHER SUBSTANCES
Simul taneous:
asp irin, benzyl alcohol, benzyl ben zoate, caffeine, calu stero ne, cortisone, de-
hydroepiandrosterone (UV 210), formebolone, mesterolone (UV 210), methandriol (UV
210), m ethandrostenolone, m ethenolone acetate, methyltestosterone, m ibolerone, nandro-
lone, nandrolone acetate, nandrolone propionate, norethandrolone, norgestrel, oxymeth-
olone, stanozolol, testolactone, testostero ne, testostero ne a cetate, testos terone propion ate,
trenbolone acetate
Interfering:
boldenone, ethisterone, fluoxymesterone, oxandrolone (UV 210)
KEYWORDS
oils;
tablets; suspensions
REFERENCE
Walters, M.J.; Ayers, R.J.; Brown, D.J. Analysis of illegally distributed anabolic steroid products by
liquid chromatography with identity confirmation by mass spectrometry or infrared spectrophotom-
etry J.Assoc.Off.Anal.Chem. 1990 73 904-926
SAMPLE
Matrix:
formulations
Sample preparat ion:
Dissolve 5 g cream con taining 0.00925 fluocinonide, 0.00365 pro-
cinonide, and 0.0021 ciprocinonide in 2.5 mL THF, add norethin dron e, dilute to 25 mL
with MeOH, centrifuge, inject a 25 JULL aliquot onto column A with mobile ph ase A and
allow com ponents to elu te from column A to column B for 7 m in. After 7 m in rem ove
column A from circuit, mo nitor effluent from column B . Back-flush column A w ith m obile
pha se B for 5 min, equ ilibrate column A with mobile ph ase A for 5 min before next
injection.
HPLCVARIABLES
Column: A 30 X 4.6 5 >jim Spheri-5 ODS (B rownlee); B 70 X 2.1 Wh atm an Co :Pell ODS +
250 X 4.6 5 |jim U ltras ph ere C18
Mobile phase: A M eCN :THF:water 4 3:4 :53 ; B MeOH :THF 75:25
Flow rate: A 1.5; B 1
Inject ion volume:
25
Detector:
UV 260 for 22 min then UV 236
CHROMATOGRAM
Retent ion t ime: 12
Internal s tandard: norethindrone
OTHER SUBSTANCES
Simul taneous: ciprocinonide, fluocinolone acetonide, fluocinonide, procinonide
KEYWORDS
creams; column-switching; norethindrone is IS
REFERENCE
Conley, D.L.; Benjamin, E.J. Automated high-performance liquid chromatographic column switching
techniqu e for the on-line clean-up and analy sis of drugs in topical cream formulations. J.Chromatogr.
1983, 257 337-344
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SAMPLE
Matrix: formulations
Sample preparat ion:
1 Tablet + 4 mL 50 mM KH
2
PO
4
, rotate 15 min, add 2 mL 1 ixg/mL
o-phenylphenol in mobile pha se, add 4 mL MeOH , rot ate 15 min , centrifuge. Remove
supernatant, extract residue twice with 5 mL mobile phase (10 min rotation), combine
supernatants, inject 50
|JLL
aliquot.
HPLC VARIABLES
Column: 250 X 4.6 10 (xm L iChrosorb RP 8
M obile pha se: MeOH:50 mM KH
2
PO
4
3:2
Flow rate: 2
Inject ion volum e: 50
De tecto r: UV 220
CHROMATOGRAM
Retent ion t ime:
9 (norethindrone), 19.3 (norethindrone acetate)
OTHER SUBSTANCES
Simul taneous:
methyltestosterone, norgestrel
Interfering: ethinyl estradiol
KEYWORDS
tablets; stability-indicating
REFERENCE
Strus iak, S.H.; Hoogerheide, J.G.; G ardner, M.S. Determ ination of ethinyl estrad iol in solid dosage forms
by high-performance liquid chromatography.
J.Pharm.Sci.
1982
71
636-640
SAMPLE
Matrix:
reaction mixtures
Sample preparat ion: If necessary, remove oxidizing power of solution by adding sodium
metabisulfite, inject a 20
JJLL
aliquot.
HPLC VARIABLES
Guard column: 15 X 4.6 5 |xm M icrosorb C8
Column:
250 X 4.6 5 |xm Microsorb C8
Mobile phase:
M eCN: 100 mM KH
2
PO
4
adjusted to pH 7 with 1 M KOH 50:5 0
Flow rate: 1
Inject ion volume: 20
Detector: UV
254
CHROMATOGRAM
Retent ion t ime: 8 .7
Limit of detect ion: 100 ng/mL
REFERENCE
L unn , G.; Rhodes, S.W.; Sanso ne, E.B.; Schmuff, N.R. Photolytic destruction and polymeric resin decon-
tamination of aqueous solutions of pharmaceuticals.
J.Pharm.Sci.
1994
83
1289-1293
SAMPLE
Matrix:
solutions
HPLCVARIABLES
Column: 50 X 4.6 5 Jim Supelcosil L C-18
Mobile phase:
MeOH : TH F: water 10:20:70
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Flow rate: 2
Inject ion volume: 20
Detector: UV 220
CHROMATOGRAM
Retent ion t ime: 3 (norethindrone), 7.4 (norethindrone acetate)
OTHER SUBSTANCES
Simul taneous: ethinyl estradiol, norethynodrel acetate, norgestrel
REFERENCE
Supelco Catalog Supelco Inc Bellefonte PA
1996, p. A130
SAMPLE
Matrix:
solutions
Sample preparat ion: Inject a 5 JJLL aliquo t of a 10 jxg/mL solution in M eOH.
HPLCVARIABLES
Column: 75 X 4.6 3 fxm U ltras ph ere ODS
Mobile phase:
MeC N: 10 mM am mon ium acetate buffer 45:5 5
Flow rate: 0 .5
Inject ion volume: 5
Detector: UV 254
CHROMATOGRAM
Retent ion t ime:
5.941
OTHER SUBSTANCES
Simul taneous: boldenone, epime thand ienon e, ep itestosterone, fluoxymesterone, 6p-hy-
droxymethandienone, methandienone, oxymetholone (UV 280), trenbolone
REFERENCE
Barron, D.; Pascual, J.A.; Segura, J.; Barbosa, J. Prediction of LC retention of steroids using solvato-
chromic parameters. Chromatographia 1995, 41 573-580
SAMPLE
Matrix: solutions
Sample preparat ion:
Inject a 20
\iL
aliquot of a solution in MeO H: w ater 50:5 0.
HPLCVARIABLES
Column:
250 X 4 7 |jim L ichroCAR T RP -8 (Merck)
Mobile phase:
MeCN: MeOH: water 32:37:31
Flow rate: 1
Inject ion vo lum e:
20
Detector: UV
230
CHROMATOGRAM
Retent ion t ime: 5
OTHER SUBSTANCES
Simul taneous: fluoxymesterone, m edrogestone, m estrano l, progesterone, tes tostero ne
propionate
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REFERENCE
Gau, YS.; Sun, S.W.; Chem, R.R.-L. Optimization of high-performance liquid chromatographic separa-
tion for progestogenic, estrogenic, and androgenic steroids usin g factorial design. J.Liq.Chromatogr.
1995, 18 2373-2382
SAMPLE
Matrix: solutions
HPLCVARIABLES
Column: 250 X 4.6 10 ^m Nucleosil C18
Mobile phase: MeCN:THF-.water 12.9:22.4:64.7
Flow rate: 1
D etecto r: UV 240
CHROMATOGRAM
Retent ion t ime:
8.5 (norethindrone), 15.5 (norethindrone acetate)
OTHER SUBSTANCES
Simul taneous:
estrone, ethinyl estradiol, mestranol, norgestrel
REFERENCE
Gazdag, M.; Szepesi, G.; Szeleczki, E. Selection of high-performance liquid chromatographic methods in
pharmaceutical analysis. I. Optimization for selectivity in reversed-phase chromatography.
J.Chromatogr.
1988
454 8 3 - 9 4
SAMPLE
Matrix: solutions
HPLCVARIABLES
Column: 250 X 4.6 5 ^m L iChrosorb Si 60
Mobile phase: Hex ane: dioxane: isopropanol 95 :3: 2
Flow rate: 1
Detector: UV 254
CHROMATOGRAM
Retent ion t ime:
20 (norethindrone), 10 (norethindrone acetate)
OTHER SUBSTANCES
Simul taneous: estrone, ethinyl estradiol, mestranol, norgestrel
KEYWORDS
normal phase
REFERENCE
Gazdag, M .; Szepesi, G.; Fabian-Varga, K. Selection of high-performance liquid chrom atographic m eth-
ods in pharmaceutical analysis. II. Optimization for selectivity in normal-phase systems.
J.Chromatogr.
1988
454 9 5 - 1 0 7
SAMPLE
Matrix: solutions
Sample preparat ion: Dissolve in MeO H: w ate r 1:1 at a conc entration of 50 |xg/mL , inject
a 10
|JLL
aliquot.
HPLCVARIABLES
Column:
300
X 3.9 10 |xm
(xBondapak C18
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Mobile phase:
MeOH: acetic acid: triethylamine: water 60:1.5:0.5:38
FIo
5
W rate: 1.5
Injection volume: 10
Detector: UV 240
CHROMATOGRAM
Retention time: 12
OTHER SUBSTANCES
Simultaneous: hydrocortisone acetate, methyltestosterone, prednisolone, prednisolone suc-
cinate, prednisone, progesterone
REFERENCE
Roos,
R.W.;
L au-Cam,
CA.
Gen eral reversed-ph ase high-performance liquid chromatograp hic method
for
the
separation
of
drugs using triethylamine
as a
competing base.
J.Chromatogr.
1986
370
403-418
• • •
ANNOTATED BIBLIOGRAPHY
Tang, G.P.; Chen, Q.Q. [Column switching H PL C method for determination of in vivo relea se of noreth-
indrone-alpha , beta-poly (3-hydroxypropyl)-DL -asparamide conjugate].
Y ao Hsueh Hsueh Pao
1994
29 301-305
Lee, G.J.-L.; Oyang, M.-H.; Bautista,
J.;
Kushinsky,
S.
Determination
of
ethinylestradiol
and
noreth-
indrone
in a
single specimen
of
plasma
by
autom ated high-performance liquid chromatograp hy
and
subsequent radioimmunoassay.
J.Liq.Chromatogr.
1987 10 2305-2318 [LOD 20-50 pg/mL ]
Papas,
A.N.;
Marchese,
S.M.;
Delaney,
M.F.
Rapid determina tion
of
norethindrone
and
ethinylestradiol
in oral contraceptive tablets
by
reversed-phase liquid chromatography.
LC
Mag.
1985
3
354-358
[tablets; column temp
25;
simultaneous ethinylestradiol; Chem.Abs.,
102,
226114]
Swynnerton, N.R; Fischer, J.B. Determination of ethyny lestradiol and norethindrone in synthetic in-
testinal fluid
and in
timed-release oral formulations.
J.Liq.Chromatogr.
1980
3
1195-1204
[for-
mulations; also ethinylestradiol]
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