Propoxyphene

7/25/2019 Propoxyphene

1/13

SAMPLE

Matrix: blood

Sample preparat ion:

2 mL Whole blood or pla sm a + 2 mL buffer + 5 mL chloroform:

isopropanol: n-h epta ne 60 :14 :26 , shak e gently horizontally for 10 min, centrifuge a t 2800

g for 10 min. Remove the lower organic layer and evaporate it to dryness under vacuum

at 45, reconstitute the residue in 100 |xL mobile phase, centrifuge at 2800 g for 5 min,

inject a 50 |JLL aliquot of th e s up ern ata nt. (Buffer w as s atu rat ed amm onium chloride

solution 25 diluted with water, adjusted to pH 9.5 with 25 amm onia solution.)

HPLCVARIABLES

Column:

300 X 3.9 4 fim NovaPack C18

Mobile phase:

M eO H:T H F:b uffe r 6 5: 5 :3 0 (Buffer w as 0.68 g/L (10 mM (sic)) KH

2

PO

4

adjusted to pH 2.6 with concentrated orthophosphoric acid.) (At the end of each session

wash the column w ith w ater for 1 h an d M eOH for 1 h, re-equilibrate for 30 min.)

Column tem pera ture: 30

Flow rate: 0.8

Inject ion volum e: 50

Detector: UV259

CHROMATOGRAM

Retent ion t ime:

7.24

Limit of detect ion:


2/13

zolam, minoxidil, moclobemide, moperone, morphine, nadolol, nalbuphine, nalorphine,

naloxone, naltrexone, naproxen, nialamide, nicardipine, nifedipine, niflumic acid, nimo-

dipine, nitrazepam, nitrendipine, nizatidine, nomifensine, nortriptyline, omeprazole,

opipramol, oxazepam, oxprenolol, penbutolol, penfluridol, pentazocine, phencyclidine,

phenobarbital, phenol, phenylbutazone, pimozide, pindolol, pipamperone, piroxicam, pra-

zepam, prazosin, prilocaine, procainamide, procarbazine, proguanil, propranolol, protrip-

tyline, pyrimetham ine, quinidine, quinine, quinup ramine , ramipril , ranitidine, reserpine,

ritodrine, secobarbital, sotalol, strychnine, sulfinpyrazole, sulindac, sulpride, sultopride,

suriclone, temazepam, tenoxicam, terbutaline, terfenadine, tetracaine, tetrazepam, thio-

pen tal, thiorida zine, tia nep tine , tiap ride, tiaprofenic acid, ticlopidine, timolol, tioclomarol,

tofisopam, to lbutam ide, toloxatone, trazodone, triazolam , trifluoperazine, trifiuperidol, tri-

mipramine, triprolidine, tropatenine, verapamil, viloxazine, vinblastine, vincristine, vin-

desine, warfarin, yohimbine, zolpidem, zopiclone, zorubicine

Interfering: betaxolol, dextromoramide, dextropropoxyphene, dosulepine, fenoprofen, lox-

apine, methadone, prom ethazine, propafenone, thioproperazine

KEYWORDS

whole blood; plasma

REFERENCE

Tracqui, A.; Kintz, P.; Mangin, P. Systematic toxicological analysis using HPLC/DAD.

J.Forensic Sci.

1995,40 254-262

SAMPLE

Matrix:

blood


Condition a 3 mL Bond Elu t Certify SPE ca rtridge with 2 mL MeOH

and 2 mL 100 mM pH 6.0 phosphate buffer, do not allow to dry. 1 mL Blood + 6 mL 100

mM pH 6.0 phos pha te buffer, vortex, sonicate, centrifuge, add the s up er na tan t to th e SP E

cartridge, wash with water, wash with 1 mM pH 3.3 acetic acid, dry by suction, wash

with 2 mL acetone: chloroform 50:50 , elute with 3 mL ethyl aceta te: amm onia 9 8:2 . Evap-

orate th e elu ate u nd er a s trea m of nitrogen at 40, reco nstitu te th e resid ue in 50 |JLL

MeOH, inject a 10 |xL aliquot.

HPLCVARIABLES

Column:

150 X 3.9 4 ^m Nova-Pack C18

Mobile phase: M eOH : 50 mM am m onium aceta te 75 :25 (Mix column effluent w ith 50 mM

ammonium acetate pumped at 0.5 mL/min.)

Flow rate: 0.6

Inject ion volume: 10

Detector: MS, Finnigan MAT TSQ 700 tandem quadrupole, MAT TSP-2 interface, ther-

mospray, selective re act ion m on itor ing m/z 340-266, collision offset -6 V, rep elle r 100 V,

vaporize r 130, source 200, filament on 200 jxA, argo n 2.5 mTorr, mu ltip lier 1500 V,

dynode 15 kV, scan time 1.20 s, MSMSC factor 10

CHROMATOGRAM

Retent ion t ime: 7.10 (dextropropoxyphene)

Limit of detection: 50

pg

OTHER SUBSTANCES

Extracted:

benperidol, dextromoramide, droperidol, haloperidol, methadone, penfluridol,

pimozide, pipamperidone

KEYWORDS

SPE; LC/MS


3/13

REFERENCE

Verweij,

A.M.A.; Hordijk, M.L.; Lipman, P.J.L. Quantitative liquid chromatographic thermospray-

tandem mass spectrometric analysis of some analgesics and tranquilizers of the methadone, butyr-

ophenone, or diphenylbutylpiperidine groups in whole blood. J.Anal.ToxicoL 1995,19 6 5 - 6 8

SAMPLE

Matrix: blood


Autom ated SP E by ASPEC system. Condition a C18 Clean-Up SP E

cartridge (CEC 18111, Worldwide Monitoring) with 2 mL MeOH then 2 mL water. 1 mL

Plasm a + 1 mL 400 ng/mL protriptyline in water, vortex, add to the S PE cartridge, wa sh

with 3 mL water, wash with 3 mL 750 mL/L methanol. Elute with three aliquots of 300

|xL 0.1 M ammonium acetate in MeOH. Add 0.5 mL 0.5 M NaOH and 4 mL 50 mL/L

isopropanol in heptane to eluate, mix thoroughly. Allow 5 min for phase separation. Re-

move upper heptane phase and add it to 300 |xL 0.1 M phosphoric acid (pH 2.5), mix,

separate, inject a 100 u,L aliquot of the aqueous phase.

HPLCVARIABLES

Guard column: LC-8-DB (Supelco)

Column:

150 X 4.6 LC-8-DB (Supelco)

Mobile phase: MeCN.buffer 35:65 (Buffer was 10 mL/L triethylamine in water adjusted

to pH 5.5 with glacial acetic acid.)

Flow rate: 2

Inject ion vo lume: 100

Detector: UV

228

CHROMATOGRAM

Reten tion tim e: 5 2

Internal s tandard:

protriptyline (4)

OTHER SUBSTANCES

Extracted:

acetazolamide, amitriptyline, chlordiazepoxide, chlorimipramine, chlorproma-

zine, desipramine, dextromethorphan, diazepam, diphenhydramine, doxepin, encainide,

fentanyl, flecainide, fluoxetine, flurazepam, haloperidol, hydroxyethylflurazepam, ibupro-

fen, imipramine, lidocaine, methaqualone, mexiletine, midazolam, norchlorimipramine,

nordoxepin, nortriptyline, norverapamil, pentazocine, promazine, propafenone, propran-

olol, protriptyline, quinidine, trazodone, trimipramine, verapamil

Noninterfer ing: acetaminophen, acetylmorphine, amiodarone, amob arbital, amphe tam ine,

bendroflumethiazide, benzocaine, benzoylecgonine, benzthiazide, butalbital, carbamaze-

pine, chlorothiazide, clonazepam, cocaine, codeine, cotinine, cyclosporine, cyclothiazide,

desalkylflurazepam, diamorphine, dicumerol, ephedrine, ethacrynic acid, ethanol, eth-

chlorvynol, ethosuximide, furosemide, glutethimide, hydrochlorothiazide, hydrocodone,

hydroflumethiazide, hydromorphone, lorazepam, mephentermine, meprobamate, meth-

amphetamine, metharbital, methoxsalen, methoxyphenteramine, methsuximide, meth-

ylcyclothiazide, metoprolol, MHPG, monoacetylmorphine, morphine, normethsuximide,

oxazepam, oxycodone, oxymorphone, pentobarbital, phencyclidine, phenteramine, phen-

ylephrine, phenytoin, polythiazide, primidone, prochlorperazine, salicylic acid, sulfanila-

mide, THC-COOH, theophylline, thiazolam, thiopental, thioridazine, tocainide, trichlo-

romethiazide, trifluoperazine, valproic acid, warfarin

Interfering: maprotiline, methadone, nordiazepam, norfluoxetine, temazepam

KEYWORDS

plasma; SPE

REFERENCE

Nichols, J.H.; Charlson, J.R.; Lawson, G.M. Automated HPLC assay of fluoxetine and norfluoxetine in

serum. Clin.Chem. 1994,40 1312-1316


4/13

SAMPLE

Matrix: blood


2 mL Whole blood + 20 jxL 100 |xg/mL meth ado ne in MeO H + 1 mL

pH 11 Normex buffer (Carlo Erba) , vortex for 20 s, add to a 3 mL Extr elut cartridge , wait

for 10 min, elute w ith diethyl eth er: dichlorom ethane 70:3 0. Add the e luate to 100 jxL 10

mM HCl and evaporate it at 40 under a stream of nitrogen. Wash the residual acid

solution with 3 mL diethyl ether, inject a 40 jxL aliquot of the aqueous phase.

HPLCVARIABLES

Guard column: 5 x 6 jxBondapak C18 Guard-Pak

Column:

300 X 3.9 10 jxm ixBondapak C18

Mobile phase: M eCN : buffer 7 5:2 5 (Buffer w as 0.1 acetic acid in 10 mM am m oniu m

acetate.)

F lo w rate: 1.5


Detector: UV215

CHROMATOGRAM

Retent ion t ime: 13.42

Internal s tandard: methadone (16.40)


40 ng/mL

OTHER SUBSTANCES

Extracted: dextromoramide, norpropoxyphene

Simul taneous: alimemazine, amitriptyline, amphetamine, bupivacaine, buprenorphine,

clomipramine, cocaine, codeine, ethylmorphine, glafenine, meperidine, methampheta-

mine, methotrimeprazine, morphine, norcodeine, nortriptyline, pentazocine

Noninterfer ing: acetaminophen, aspirin, barbiturates, benzoylecgonine, caffeine, diaze-

pam, fiunitrazepam, lidocaine, lorazepam, nalorphine, naloxone, nitrazepam, nordiaze-

pam, norflunitrazepam, normorphine, oxazepam, prazepam, triazolam, zolpidem

Interfering: cyamemazine, desipramine, imipramine

KEYWORDS

whole blood

REFERENCE

Rop,

P.P.; Grimaldi, R; Bresson, M.; Fornaris, M.; Viala, A. Simultaneous determination of dextromo-

ramide, propoxyphene and norpropoxyphene in necropsic whole blood by liquid chromatography.

J.Chromatogr. 1993 615 357-364

SAMPLE

Matrix: blood

Sample preparat ion: 1 mL Pla sm a + 20 jxL 20 (xM IS in w ate r + 300 |JLL 100 mM p H

10.0 sodium carbonate buffer + 4 mL n-hex ane : diethyl eth er: n-butan ol 7 0: 25 :5 , rotate

gently for 10 min, centrifuge at 3200 g at 2 for 10 min. Remove the organic layer and

add it to 250

|JLL

pH 2.0 phosphate buffer, vortex for 15 s, centrifuge, inject 175 jxL of the

aqueous layer.

HPLC VARIABLES

Column: 100 X 4.6 YMC S-3 120A ODS (YMC)

Mobile phase:

MeC N:buffer 39.5:60.5 + 0.2 mM N, N-dim ethyloctylamine + 1 mM sodium

decyl sulfate (Buffer was 50 mM NaH

2

PO

4

adjusted to pH 2.0 with orthophosphoric acid.)

Flow ra te: 1.3


Detector: UV

210


5/13

CHROMATOGRAM

Retent ion t ime: 6

Internal s tandard: l-benzyl-3-methylethylamm o-2-methyl-l-phenylpropy l prop ionate pic-

rate (7.5)

Lim it of qua ntitatio n: 2 nM

OTHER SUBSTANCES

Extracted:

norpropoxyphene

KEYWORDS

plasma

REFERENCE

Pettersson, K.J.; Nilsson, L.B. Determination of dextropropoxyphene and norpropoxyphene in plasma

by high-performance liquid chromatography

J.Chromatogr.

1992

581

161

164

SAMPLE

Matrix: blood


1 mL Ser um + 200 ng doxepin or des ipra m ine H- 500 jxL 2 pH 9.5

sodium tetra bo rate + 9 mL freshly prep ared hex an e: isoamyl alcohol 9 9 :1 , sha ke vigor-

ously for 5 min, centrifuge. Remove 8.5 mL of the organic phase and add it to 200 |xL 50

mM HCl, shake well for 1 min, centrifuge, inject a 50 |JLL aliquot of the aqueous phase.

HPLC VARIABLES

Column:

300 X 4 ixBondapak phenyl

Mobile phase: MeC N: 0.01 phosphoric acid containing 0.01 NaC l 35 :65 , final pH 2.8

Flow ra te:

1.5


Detector: UV210

CHROMATOGRAM

Retention t ime: 18.6

Internal s tandard: doxepin (12.2), desipramine (14.2)

Limit of detect ion: 10 ng/mL

OTHER SUBSTANCES

Extracted: cocaine, dextromoramide, meperidine, methadone, normeperidine, norpropoxy-

phene, pentazocine

Simul taneous: amitriptyline, buprenorphine, chlorpromazine, codeine, desmethyldoxepin,

diphenhydramine, ephedrine, imipramine, nortriptyline, oxazepam, oxycodone, pericy-

azine, pheniramine, propranolol, quinine, thiopropazate, thioridazine

KEYWORDS

serum

REFERENCE

Hackett, L.P.; Dusci, L.J.; Ilett, K.F. The analysis of several nonopiate narcotic analgesics and cocaine

in serum using high-performance liquid chromatography.

J.Anal.ToxicoL

1987

11

2 6 9 - 2 7 1

SAMPLE

Matrix: blood, CSF

Sample preparat ion: 200 |xL Serum , plasm a, or CSF + 300 JJLLreagent. Flush column A

to waste with 500 |xL 500 mM ammonium sulfate, inject sample onto column A, flush

column A to waste w ith 500 |xL 500 mM am mo nium sulfate, elute th e conte nts of column


6/13

A onto column B with mobile phase, monitor the effluent from column B. (Reagent was

8.05 M guanidine HCl and 1.02 M ammonium sulfate in water.)

HPLCVARIABLES

Column: A 30 X 2.1 40 \xm preparative grade C18 (Analytichem); B 250 X 4.6 10 [xm

Partisil C8

Mobile phase:

Gradient. A was 50 mM pH 4.5 KH

2

PO

4

. B w as M eCN: isopropanol 80:20 .

A :B 9 0:10 for 1 min, to 30:70 over 15 min, m ain tain at 30 :70 for 4 min.

Colum n tem peratu re: 50

Flow rate: 1.5

Detector:

UV 280 for 5 min then UV 254

CHROMATOGRAM

R ete nt ion t ime: 6.96

Internal s tandard: heptanophenone (19.2)

OTHER SUBSTANCES

Extracted: acetazolamide, ampicillin, brom azepam , caffeine, carbamaz epine, chloram phen-

icol, chlorothiazide, diazepam, droperidol, ethionam ide, furosemide, isoniazid, m ethad one,

penicillin G, phenobarbital, phenytoin, prazepam, pyrazinamide, rifampin, trimeprazine,

trimethoprim

KEYWORDS

serum; plasma; column-switching

REFERENCE

Seifart, H.I.; Kruger, RB.; Parkin, D.R; van Jaarsveld, P.P.; Donald, RR. Therapeutic monitoring of

antitube rculosis drug s by direct in-line extraction on a high-performance liquid chromatog raphy sys-

tem.J.Chromatogr. 1993,619 285-290

SAMPLE

Matrix:

blood, CSF, gastric fluid, urine

Sample preparat ion: 200 |xL Se rum , urin e, CSF, or gas tric fluid + 300 |xL rea ge nt. Flu sh

column A to waste with 500

JJLL

500 mM am mo nium sulfate, inject s am ple onto column

A, flush column A to was te wit h 500 |xL 500 mM am mo nium sulfate, back flush th e con-

tents of column A onto column B with mobile phase, monitor the effluent from column B.

(Reagent was 8.05 M guanidine hydrochloride and 1.02 M ammonium sulfate in water.)

HPLCVARIABLES

Column:

A 40 |xm preparative grade C18 (Analytichem); B 75 X 2.1 pellicular C18 (What-

ma n) + 250 X 4.6 5 fim C8 end-capped (W hatman)

Mobile phase: Gradient. A was 50 mM pH 4.5 KH

2

PO

4

. B was M eCN: isopropanol 80:2 0.

A :B 90:10 for 1 min, to 30:70 over 20 min.

Colum n tem peratu re: 50

Fl ow rate: 1.5

Detector: UV220

CHROMATOGRAM


Internal s tandard:

heptanophenone (19)

OTHER SUBSTANCES

Extracted: acetaminophen, allobarbital, azinphos, barbital, brallobarbitone, bromazepam,

butethal, caffeine, carbamazepine, carbaryl, cephaloridine, chloramphenicol, chlordiaze-

poxide, chlorothiazide, chlorvinphos, clothiapine, cocaine, coomassie blue, desipramine,

diazepam, diphenhydramine, dipipanone, ethylbromphos, flufenamic acid, formothion,


7/13

griseofulvin, indom ethacin, lidocaine, lorazepam , m alathion , med azepam , midazolam , ox-

azepam, paraoxon, penicillin G, pentobarbital, prazepam, prothiophos, quinine, salicylic

acid, secobarbital, strychnine, sulfamethoxazole, theophylline, thiopental, thioridazine,

trimethoprim

KEYWORDS

serum; column-switching

REFERENCE

Kruger, RB .; Albrecht, C.F.De V.; Jaa rsve ld, P.P. Use of guan idine hydrochloride and am mon ium sulfate

in comprehensive in-line sorption enrichment of xenobiotics in biological fluids by high-performance

liquid chromatography.

J.Chromatogr.

1993

612

191-198

SAMPLE

Matrix:

blood, milk

Sample preparat ion: Adjust 0.2-1 mL plasm a or bre ast m ilk to 1 mL with blank biological

fluid if necessary, add 50 jxL 12 |xg/mL IS in EtOH, add 500

\xL

1 M pH 9.80 carbon ate:

bicarbonate buffer, add 10 mL n-butyl chloride, shake at high speed on a reciprocating

shaker for 15 min, centrifuge at 2000 g for 5 min. Remove the organic phase and add it

to 5 mL 200 mM HC l, sha ke at high speed on a reciprocating sh aker for 15 min , centrifuge

at 2000 g for 5 min. Remove the aqueous phase and wash it with 5 mL ether. Add 500

IxL 4 M NaO H to the aqueou s ph ase , add 10 mL chloroform, shak e a t high speed on a

reciprocating sh ake r for 15 m in, centrifuge at 2000 g for 5 min. Remove the organic p has e

and evaporate it to dryness under nitrogen at 55, dissolve the residue in 200 fxL mobile

phase, inject a 100 JJLLaliquot.

HPLCVARIABLES

Column: 300 X 3.9 [iBond apak C 18

Mobile phase: M eCN : 2 mM sulfuric acid 50:5 0

Flow ra te:

1.5

Inject ion vo lum e: 100

Detector: UV205

CHROMATOGRAM

Retent ion t ime: 5 .7

Internal s tandard:

2-diethylaminoethyl-2,2-diphenylvalerate hydrochloride (SKF 525-A)

(8.8)


20 ng/mL

OTHER SUBSTANCES

Extracted:

norpropoxyphene

KEYWORDS

plasma; breast

REFERENCE

Kunka, R.L.; Yong, C-L.; Ladik, CR; Bates, T.R. Liquid chromatographic determination of propoxy-

phene and norpropoxyphene in plasma and breast milk.

J.Pharm.ScL

1985

74

103-104

SAMPLE

Matrix:

blood, tissue


Blood. 1 mL Whole blood or serum + 1 |xg cianopramine 4- 1 mL

water, vortex, add 1 mL 200 mM sodium carbonate, vortex, add 6 mL hexane: 1 butanol

95:5 , gently agitate for 30 min, centrifuge at 2500 g for 5 min. Remove the organic layer

and add it to 100 jxL 0.2 pho spho ric acid, agita te gently for 30 min , centrifuge for 5

min. Remove the organic layer and inject a 30 |xL aliquot of the aqueous layer. Tissue.


8/13

0.5 mL Liver homogenate + 10 \xgcianopram ine + 500 |xL 2 sodium tetr ab ora te + 8

mL hexane:l-butanol 95:5, gently agitate for 30 min, centrifuge at 2500 g for 5 min.

Remove the organic layer and add it to 400 JJLL0.2 phosphoric acid, ag itat e gently for

30 min, centrifuge for 5 min. Remove the organic layer and inject a 30 |xL aliquot of the

aqueous layer.

HPLC VARIABLES

Guard co lumn:

15 X 3.2 7 |xm RP-18 Newguard (Applied Biosystems)

Column: 100 X 4.6 5 fxm Brownlee Spheri-5 RP-18

Mobile phase: MeC N: 100 mM NaH

2

PO

4

: diethylamine 40:57 .5:2.5

Flow rate: 2


Detector: UV220

CHROMATOGRAM

Retention time: 12 76

Internal s tandard:

cianopramine (8.93)

OTHER SUBSTANCES

Extracted: amitriptyline, amoxapine, benztropine, brompheniramine, chlorpheniramine,

chlorpromazine, clomipramine, cyproheptadine, desipramine, diphenhydramine, dothie-

pin, doxepin, fluoxetine, haloperidol, imipramine, loxapine, maprotiline, meperidine,

me thado ne, metoclopramide, m ianse rin, m oclobemide, nomifensine, nordoxepin, norfluox-

etine, norpropoxyphene, northiaden, nortriptyline, pentobarbital, pheniram ine, prometh-

azine, propranolol, protriptyline, quinidine, quinine, sulforidazine, thioridazine, thiothix-

ene,

tranylcypromine, trazodone, trihexyphenidyl, trim ipram ine, triprolidine

Noninterfer ing:

dextromethorphan, norphetidine, phenoxybenzamine, prochlorperazine,

trifluoperazine

Interfering: mesoridazine

KEYWORDS

whole blood; serum; liver

REFERENCE

Mclntyre, LM.; King, CV.; Skafidis, S.; Drummer, O.H. Dual ultraviolet wavelength high-performance

liquid chromatographic method for the forensic or clinical analysis of seventeen antidepressants and

some selected metabolites.J.Chromatogr. 1993,621 2 1 5 - 2 2 3

SAMPLE

Matrix:

blood, tissue


2 mL Blood or 250 mg liver (homogenized with 3 parts water) or

500 mg brain (homogenized with 3 parts water) + 2 jig SKF-525-A + 1.5 mL pH 9.5

amm onium carbonate/ammonium hydroxide buffer + 1 0 mL hexan e: isopropanol 99 :1 ,

rotate at 10 rpm for 10 min, centrifuge at 3500 rpm for 10 min. Remove the organic layer

and add it to 2.5 mL 0.25 M sulfuric acid, rotate for 5 min, centrifuge at 1500 rpm for 5

min. Remove the aqueous layer and add concentrated ammonium hydroxide to make the

pH 9.5, add 1.5 m L chloroform, v ortex for 15 s, centrifuge at 1500 rpm for 5 m in. Remove

th e organic layer and add 1 drop of 1 HCl in MeOH, evaporate to dryne ss at 50 un der

vacuum, reconstitute with 200 |JLL mobile phase, inject a 100 |JLL aliquot.

HPLCVARIABLES

Guard co lumn:

30 X 2.1 Whatman C18 pellicular

Column: 250 X 4.6 Sp heriso rb S-5-ODS

Mobile phase:

MeCN :MeO H:buffer 48 :4 :4 8 (Buffer w as 1980 mL water + 20 mL 85

phosphoric acid + 3.7 mL methanesulfonic acid adjusted to pH 3.0 with 5 M NaOH.)

Column temp erature: 60

Flow rate: 2


9/13

Injection volume:

100

Detector: UV

220

CHROMATOGRAM

Retention time: 6.0

Internal standard: SKF-525-A(11.2)

Limit of quantitation: 100 ng/mL

OTHER SUBSTANCES

Extracted: N-desmethyldiazepam, diazepam, methadone, norpropoxyphene

KEYWORDS

liver; brain

REFERENCE

Rio,

J.; Hodnett, N.; Bidanset, J.H. The determination of propoxyphene, norpropoxyphene, and metha-

done in postmortem blood and tissues by high-performance liquid chromatography J.AnaLToxicoL

1987

11

222-224

SAMPLE

Matrix:

formulations

Sample preparation: Add one tablet to 10 mL MeOH and 80 mL dichloromethane, soni-

cate for 5 min, dilute to 100 mL with dichloromethane, dilute a 2 mL aliquot to 25 mL

with mobile phase, inject a 10 |xL aliquot.

HPLCVARIABLES

Guard column:

20 X 4.6 5 jxm Supelcosil

Column:33 X 4.6 3 |xm Supelcosil

Mobile phase:

Dichloromethane:3.33 ammonium hydroxide in MeOH 98.5:1.5

Flow rate: 2

Injection volume: 10

Detector: UV244

CHROMATOGRAM

Retention time: 2

Limit of detection: 2500 ng/mL

OTHER SUBSTANCES

Simultaneous:

acetaminophen

Noninterfering:

impurities, 4-aminophenol, p-hydroxyacetophenone, p-nitrophenol

KEYWORDS

tablets; normal phase

REFERENCE

Ascah, T.L.; Hunte r, B.T. Sim ultaneo us h igh-performance liquid chrom atographic d eterm ination of pro-

poxyphene and acetaminophen in pharmaceutical preparations.J.Chromatogr.

1988

455 279-289

SAMPLE

Matrix:

solutions

H P L C V A R I A B L E S

Column:

250 X 4.6 Zorbax RX

Mobile phase:

Gradient. A was 10 mL concentrated orthophosphoric acid and 7 mL trie-

thylamine in 1 L water. B was 10 mL concentrated orthophosphoric acid and 7 mL trie-


10/13

thylamine in 200 mL water, make up to 1 L with MeCN. A:B from 100:0 to 0:100 over

30 min, maintain at 0:100 for 5 min.

Column temp erature: 30

Flow rate: 2

D etector : UV 210

OTHER SUBSTANCES

Also analyzed: acepromazine, acetaminophen, acetophenazine, albuterol, aminophylline,

amitriptyline, amobarbital, amoxapine, amphetamine, amylocaine, antipyrine, aprobar-

bital, as pirin, atenolol, atropin e, averm ectin, bar bital, benzocaine, benzoic acid, benzotro-

pine, benzphetamine, berberine, bibucaine, bromazepan, brompheniramine, buprenor-

phine, buspirone, butabarbital, butacaine, butethal, caffeine, carbamazepine, carbromal,

chloramphenicol, chlordiazepoxide, chloroquine, chlorothiazide, chloroxylenol, chlorphe-

nesin, chlorpheniramine, chlorpromazine, chlorpropamide, chlortetracycline, cimetidine,

cinchonidine, cinchonine, clenbuterol, clonazepam, clonixin, clorazepate, cocaine, codeine,

colchicine, cortisone, coumarin, cyclazocine, cyclobenzaprine, cyclothiazide, cyheptamide,

cymarin, danazol, danthron, dapsone, debrisoquine, desipramine, dexamethasone, dex-

tromethorphan, diamorphine, diazepam, diclofenac, diethylpropion, diethylstilbestrol, di-

flunisal, digitoxin, digoxin, diltiazem, diphenhydramine, diphenoxylate, diprenorphine,

dipyrone, disulfiram, dopamine, doxapram, doxepin, dronabinol, ephedrine, epinephrine,

epinine, estradiol, estriol, estrone, ethacrynic acid, ethosuximide, etonitazene, etorphine,

eugenol, famotidine, fenbendazole, fencamfamine, fenoprofen, fenproporex, fentanyl, flu-

bendazole, flufenamic acid, flunitrazepam, 5-fluorouracil, fluoxymesterone, fluphenazine,

furosemide, gentisic acid, gitoxigenin, glipizide, glunixin, glutethimide, glybenclamide,

guaiacol, halazepam, haloperidol, hydrochlorothiazide, hydrocodone, hydrocortisone, hy-

dromorphone, hydroxyquinoline, ibogaine, ibuprofen, iminostilbene, imipramine, indo-

methacin, isocarbostyril, isocarboxazid, isoniazid, isoproterenol, isoxsuprine, ivermectin,

ketamine, ketoprofen, kynurenic acid, levorphanol, lidocaine, lorazepam, lormetazepam,

loxapine, mazindol, mebendazole, meclizine, meclofenamic acid, medazepam, mefenamic

acid, megestrol, mepacrine, meperidine, mephentermine, mephenytoin, mephesin, me-

phobarbital, mepivacaine, mescaline, mesoridazine, methadone, methamphetamine,

methapyrilene, methaqualone, methazolamide, methocarbamol, methoxamine, methsux-

imide, methyl salicylate, methyldopa, methyldopamine, methylphenidate, methylpredni-

solone, methyltestosterone, methyprylon, metoprolol, mibolerone, morphine, nadolol, na-

lorphine, naloxone, naltrexone, naphazoline, naproxen, nefopam, niacinamide, nicotine,

nicotinic acid, nifedipine, niflumic acid, nitrazepam, norepinephrine, nortriptyline, nos-

capine, nylidrin, oxazepam, oxycodone, oxymorphone, oxyphenbutazone, oxytetracycline,

papaverine, pargyline, pemoline, pentazocine, pentobarbital, persantine, phenacetin,

phenazocine, phenazopyridine, phencyclidine, phen dime trazine, phenelzine, ph eniram ine,

phenobarbital, phenothiazine, phensuximide, phentermine, phenylbutazone, phenyle-

phrine, phenylpropanolamine, piperocaine, prazepam, prednisolone, primidone, probene-

cid, progesterone, propiomazine, propranolol, propylparaben, pseudoephedrine, puromy-

cin, pyrilamine, pyrithyldione, quazepam, quinaldic acid, quinidine, quinine, ranitidine,

recinnamine, reserpine, resorcinol, saccharin, albuterol, salicylamide, salicylic acid, sco-

polamine, scopoletin, secobarbital, strych nine, sulfacetamide, sufadiazine, sulfadimethox-

ine,

sulfaethidole, sulfamerazine, sulfamethazine, sulfamethoxizole, sulfanilamide, sul-

fapyridine, sulfasoxizole, sulindac, tamoxifen, temazepam, testosterone, tetracaine,

tetracycline, tetramisole, thebaine, theobromine, theophylline, thiabendazole, thiamine,

thiamylal, thiobarbituric acid, thioridazine, thiosalicylic acid, thiothixene, thymol, tola-

zamide, tolazoline, tobutamide, tolmetin, tranylcypromine, triamcinolone, tribenzylamine,

trichloromethiazide, trifluoperazine, trihexyphenidyl, trimethoprim, tripelennamine,

triprolidine, tropacocaine, tyramine, verapamil, vincamine, warfarin, yohimbine,

zoxazolamine

REFERENCE

Hill,

D.

W.;Kind,

A.

J. R eversed-phase solvent gradien t HPLC re tentio n indexes of drug s. J.Anal.ToxicoL

1994, 18 233-242


11/13

SAMPLE

Matrix: solutions

HPLCVARIABLES

Column:

300 X 3.9 (xBondapak C18

Mobile phase:

MeCNrIO mm KH

2

PO

4

+ 5 mM

1 decanesulfonic

acid: heptylamine 50:5 0:

0.1, pH adjusted to 7.9 w ith 85 pho spho ric acid

Flow rate: 2


De tector : UV 220

CHROMATOGRAM


Internal s tandard:

papaverine (2.7)


50 ng/mL

KEYWORDS

stability-indicating

REFERENCE

Ibrahim, R B. Simultaneous determina tion an d separa tion of several barb iturate s and analgesic products

by ion-pair high-performance liquid chromatography. J.Liq.Chromatogr. 1993,16 2835-2851

SAMPLE

Matrix:

solutions


Prepare a 10 |xg/mL solution in MeOH, inject a 20 |xL aliquot.

HPLCVARIABLES

Column: 125 X 4.9 Spheriso rb S5W silica

Mobile phase: MeOH containing 10 mM amm onium perchlorate and 1 mL/L 100 mM

NaOH in MeOH, pH 6.7

Flow rate: 2

Inject ion vo lum e: 20

Detector:

E, LeCarbone, V25 glassy carbon electrode, + 1.2 V

CHROMATOGRAM

Retent ion t ime:

2.5

OTHER SUBSTANCES

Also analyzed:

acebutolol, acepromazine, acetophenazine, N-acetylprocainamide, albu-

terol, alprenolol, ametbocaine, amiodarone, amitriptyline, antazoline, atenolol, azacy-

clonal, bamethane, benactyzine, benperidol, benzethidine, benzocaine, benzoctamine,

benzphetamine, benzquinamide, bromhexine, bromodiphenhydramine, bromperidol,

brompheniramine, brompromazine, buclizine, bufotenine, bupivacaine, buprenorphine,

butacaine, butethamate, chlorcyclizine, chlorpheniramine, chlorphenoxamine, chlorpren-

aline, chlorpromazine, chlorprothixene, cimetidine, cinchonidine, cinnarizine, clemastine ,

clomipramine, clonidine, cocaine, cyclazocine, cyclizine, cyclopentamine, cyproheptadine,

deserpidine, desipramine, dextromoramide, dicyclomine, diethylcarbamazine, diethylpro-

pion, diethylthiambutene, dihydroergotamine, dimethindene, dimethothiazine, diphen-

hydramine, diphenoxylate, dipipanone, diprenorphine, dipyridamole, disopyramide, doth-

iepin, doxapram, doxepin, doxylamine, droperidol, ephedrine, ergocornine, ergocristine,

ergocristinine, ergocryptine, ergometrine, ergosine, ergosinine, ergotamine, ethopropa-

zine,

etorphine, etoxeridine, fenethazine, fenfluramine, fenoterol, fentanyl, flavoxate, fluo-

promazine, flupenthixol, fluphenazine, flurazepam, haloperidol, hydroxyzine, hyoscine,

ibogaine, imipramine, indapamine, iprindole, isothipendyl, isoxsuprine, ketanserin, lau-

danosine, lidocaine, lofepramine, loxapine, maprotiline, mecamylamine, meclophenoxate,


12/13

meclozine, medazepam, mephentermine, mepivacaine, meptazinol, mepyramine, mesori-

dazine, metaraminol, methadone, methamphetamine, methapyrilene, methdilazene,

methotrimeprazine, methoxamine, methoxyphenamine, methoxypromazine, methyle-

phedrine, methylergonovine, methysergide, metoclopramide, metopimazine, metoprolol,

mianserin, morazone, nadolol, nalorphine, naloxone, naphazoline, nicotine, nifedipine,

nomifensine, nortriptyline, noscapine, orphenadrine, oxeladin, oxprenolol, oxymetazolin,

papaverine, pargyline, pecazine, penbutolol, pentazocine, penthienate, pericyazine,

perphenazine, phenadoxone, phenampromide, phenazocine, phenbutrazate, phendimetra-

zine, phenelzine, phenglutarimide, phenindamine, pheniramine, phenmetrazine, pheno-

morphan, phenoperidine, phenothiazine, phenoxybenzamine, phentolamine, phenyle-

phrine, phenyltoloxamine, physostigmine, piminodine, pimozide, pindolol, pipamazine,

pipazethate, piperacetazine, piperidolate, pipradol, pirenzepine, piritramide, pizotifen,

practolol, pramoxine, prazosin, prenylamine, prilocaine, primaquine, proadifen, procain-

amide, procaine, prochlorperazine, procyclidine, proh eptazin e, prolin tane, prom azine, pro-

methazine, pronethalol, properidine, propiomazine, propranolol, prothipendyl, protripty-

line, proxymetacaine, pseudoephedrine, pyrimethamine, quinidine, quinine, ranitidine,

rescinnamine, sotalol, tacrine, terazosin, terbutaline, terfenadine, thenyldiamine, theoph-

ylline, thiethylperazine, thiopropazate, thioproperazine, thioridazine, thiothixene, thon-

zylamine, timolol, tocainide, tolpropamine, tolycaine, tranylcyprom ine, trazodo ne, trifluo-

perazine, trifluperidol, trimeperidine, trimep razine, trimethobenz amide, trimethoprim ,

trimipramine, tripelennamine, triprolidine, tryptamine, verapamil, xylometazoline

REFERENCE

Ja ne , L; McKinnon, A.; Flan aga n,R.J. High-performance liquid chrom atographic analy sis of basic drug s

on silica columns using non-aqueous ionic eluents. IL Application of UV, fluorescence and electro-

chemical oxidation detection.

J.Chromatogr.

1985

323

191-225

SAMPLE

Matrix:

solutions

Sample preparat ion: Dissolve in MeOH at a con centra tion of 1 mg/m L, inject a 20 jxL

aliquot.

HPLCVARiABLES

Column:

250 X 5 Spherisorb S5W

Mobile phase: M eOH : buffer 90:1 0 (Buffer was 94 mL 35 amm onia and 21.5 mL 70

nitric acid in 884 mL water, adjust the pH to 10.1 with ammonia.)

Flow rate: 2


Detector: UV

254

CHROMATOGRAM

Retent ion t ime:

1.57

OTHER SUBSTANCES

Simul taneous: acetylcodeine, amphetamine, benzylmorphine, bromo-STP, chlorphenter-

min e, codeine, codeine-N-oxide, diam orphine, dihydrocodeine, dihydrom orphine, dimethy-

lamphetamine, dipipanone, ephedrine, epinephrine, ethoheptazine, ethylmorphine,

fencamfamin, fenfluramine, hydrocodone, 4-hydro xyam phetam ine, hydroxy pethidine, lev-

allorphan, levorphanol, meperidine, mephentermine, mescaline, methadone, metham-

phetamine, methylenedioxyamphetamine, methylephedrine, methylphenidate, monoace-

tylmorphine, morphine, morphine-3-glucuronide, morphine-N-oxide, norcodeine,

norlevorphanol, normetanephrine, normethadone, normorphine, norpethidine, norpipa-

none, norpseudoephedrine, oxycodone, pentazocine, phenelzine, 2-phenethylamine, phen-

termine, phenylephrine, phenylpropanolamine, pholcodine, pipradol, prolintane, pseudoe-

phedrine, STP, thebacon, thebaine, trimethoxyamphetamine, tyramine

Noninterfer ing:

dopamine, levodopa, methyldopa, methyldopate, norepinephrine


13/13

Interfering: ben zphe tam ine, bupren orph ine, caffeine, dextrom oram ide, diethylpropion,

etorphine, fenethyline, fentanyl, mazindol, nalorphine, naloxone, noscapine, papaverine,

pemoline, phenazocine, phendim etrazine, phenoperidine, piritramide, tranylcypromine

REFERENCE

Law, B.; Gill, R.; Moffat, A.C. High-performance liquid chromatography retention data for 84 basic drugs

of forensic interest on a silica column using an aqueous methanol eluent. J.Chromatogr. 1984 301

165-172

ANNOTATED BIBLIOGRAPHY

Kinney, CD.; Kelly, J.G. Liquid chromatographic determination of paracetamol and dextropropxyphene

in plasma.

J.Chromatogr.

1987

419

433-437 [verapamil (IS); electrochemical detection; column

temp 30; LOD 2 ng/mL; pharmacokinetics]

Lurie, LS.; McGuiness, K. The quantitation of heroin and selected basic impurities via reversed pfyase

HPLC. II. The an alysis of adulterated samples. J.Liq.Chromatogr. 1987 10 218 9-22 04 [UV detec-

tion; electrochemical detection; also acetaminophen, acetylcodeine, acetylmorphine, acetylprocaine,

amino pyrene, a m itriptyline, antipy rene, a spirin, barbita l, benztropine , caffeine, cocaine, codeine, dia-

morphine, diazepam, diphenhydramine, dipyrone, ephedrine, ethylmorphine, lidocaine, meconin,

methamphetamine, methapyrilene, methaqualone, monoacetylmorphine, morphine, nalorphine, nia-

cinamide, noscapine, papaverine, phenacetin, phenmetrazine, phenobarbital, phenolphthalein, pro-

caine, pyrilamine, quinidine, quinine, salicylamide, salicylic acid, secobarbital, strychnine, tartaric

acid, tetracaine, the baine, tripelenna mine , tropacocaine, vitamin B3, vitam in B5]

Schill, G.; Wainer, LW.; Barkan, S.A. Chiral separation of cationic drugs on an al-acid glycoprotein

bonded stationary phase. J.Liq.Chromatogr. 1986 9 641-666 [chiral; also atropine, bromdiphen-

hydramine, brompheniramine, bupivacaine, butorphanol, carbinoxamine, chlorpheniramine, clidi-

nium , cocaine, cyclopentolate, dimeth indene , diperidone, disopyramide, doxylamine, ephedrin e, hom-

atropine, labetalol, labetalol A, labetalol B, mepensolate, mepivacaine, methadone, methorphan,

methylatropine, methylhomatropine, methylphenidate, metoprolol, nadolol, nadolol A, nadolol B, ox-

prenolol, oxyphencyclimine, phenmetrazine, phenoxybenzamine, promethazine, pronethalol, pro-

pranolol, pseudoephedrine, terbutaline, tocainide, tridihexethyl]

Wong,S.H.Y.;McHugh, S.L.; D olan, J.; Cohen, K.A. Tricyclic antid epr essa nt analy sis by reversed -phase

liquid chromatography using phenyl columns. J.Liq.Chromatogr

1986

9 2511-2538 [also aceta-

minophen, amitriptyline, amobarbital, amoxapine, barbital, chlordiazepoxide, chlorpromazine, ci-

metidine, clomipramine, codeine, desipramine, desmethyldoxepin, diazepam, doxepin, fluphenazine,

fmrazepam, glutethimide, hydroxyamoxapine, imipramine, internal standard, lorazepam, maproti-

line, meperidine, metabolites, nortriptyline, oxazepam, pentobarbital, perphenazine, phenobarbital,

phenytoin, protriptyline, secobarbital, thioridazine, trazodone]

Angelo, H.R.; Kranz, T.; Strom, J.; Thisted, B .; Bredg aard, M. High-performance liquid ch roma tographic

method for the determination of dextropropxyphene and nordextropropoxyphene in serum.

J.Chromatogr

1985

345 413-418 [pyrroliphene (IS); LOD 100 nM; simultaneous clomipramine,

clopenthixol, codeine, ketobem idone, levomepromazine, m eperidine, m ethad one; non-interfering acet-

aminophen, amitriptyline, aprobarbital, barbital, carbamazepine, chlordiazepoxide, chlorpromazine,

chlorprothixene, desimipramine, diazepam, disopyramide, flupenthixol, imipramine, lidocaine, meth-

adone, morphine, nitrazepam, nortriptyline, oxazepam, phenobarbital, phenytoin, theophylline,

thioridazine]

Propoxyphene

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