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naproxen as crystals (mp 53°) (Pharm.Res. 1990, 7, 1262). Dissolve 1 mmole

 1,1-thiocar-

bonyldiimidazole in 15 mL ice-cold chloroform, sti r at 0°, add drop wise 1 mm ole of th e

amine dissolved in 10 mL chloroform, stir at room temperature for 1.5 h, evaporate to

dryne ss, recon stitute with carbon tetrachlo ride (Caution Carbon tetrachlor ide is a car-

cinogen ), filter, evaporate the filtrate to dryness, store the resulting oil in a desiccator,

purify on a sho rt silica gel column w ith d ichloro me thane : light petroleum 50:5 0 to give

l-(6-methoxy-2-naphthyl)ethyl isothiocyanate as a slightly yellow liquid (store in the

freezer under argon).)

HPLCV RI BLES

Column:  250 X 4 5 (xm Zorbax ODS

Mobile phase:

  MeCN: water 55:45

Flow rate: 1

Inject ion vo lume:

  100

Detector: UV  230; F  ex 270 em 350

CHROM TOGR M

Retent ion t ime: k

20.4

  (S-(-)),

  25.4

  (R-(+))

KEYWORDS

derivatization; chiral; F not much more sensitive than UV; a = 1.25

REFERENCE

Buschges, R.; Linde, H.; Mu tschler, E.; Spahn -Lan ggu th, H . Chloroformates a nd isothiocyan ates derived

from 2-arylpropionic acids as chiral reagents: synthetic routes and chromatographic behaviour of

the derivatives. J.Chromatogr.A 1996,  725 3 2 3 - 3 3 4

SAMPLE

Matrix:  solutions

HPLCV RI BLES

Column:  250 X 4.6 CSP-4 (Prepare as follows. Add a solution of 1.07 g L-valyl-L-valyl-L-

valine isopropylester (Bunseki Kagak u 1979, 28, 125) in 30 mL dry dioxane (Caution Di-

oxane is a carcinogen ) dropwise to a mixture of 2.2 g 2,4,6-trichloro-l,3,5-triazine (cyanuric

chloride) in 20 mL dry dioxane stirred at 0°, add 3 g anhydrous sodium carbonate at room

temperature, stir, filter, evaporate to give a colorless solid. Dissolve 8.3 g of this solid in 30

mL dry dioxane, add 2 g N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, add 1.5 g an-

hydrous sodium carbonate, reflux with stirring for 40 h, filter, add 3 g dried 10 |xm Li-

Chrosorb Si 100, reflux with slow stirring for 1Oh, cool, filter. Wash the solid with dioxane,

MeOH, and diethyl ether, dry under reduced pressure (J.Chromatogr. 1984, 292, 427).)

Mobile phase:

  He xan e: 1,2-dichloroethane: E tO H : trifluoroacetic acid 62 .5:35 :0.62 5:0.2 5

Detector: UV

CHROM TOGR M

Retent ion t ime:

  k/ 1.22 (first* en an tio m er)

KEYWORDS

chiral; a = 1.05

REFERENCE

Oi, N.; Kita hara , H.; M atsu shita , Y.; Kisu, N. En antio m er sepa ration by gas and high-performance liquid

chromatography with tripeptide derivatives as chiral stationary phases. J.Chromatogr.A 1996, 722

229-232

SAMPLE

Matrix:

  solutions

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HPLC V RI BLES

G ua rd colu m n: 10 X 3.2 5 |xm Partisil 0DS3

Column: 100 X 4.6 5 jxm Partisil 0DS3

M obile p hase : MeCN: buffer 25:75 (Buffer was 60 mM KH

2

PO

4

  adjusted to pH 3.0 with

phosphoric acid.)

Flow rate: 0.6-1

Injection volume: 10-100

D etec tor: UV 270

OTHER SUBSTANCES

Also analyzed: oxprenolol

REFERENCE

Palm , K.; Lu thm an, K.; Ungell, A.-L.; Stran dlun d, G.; Arturs son, P. Correlation of dru g absorption with

molecular surface properties.  J.Pharm.Sci.

1996,

 85 3 2 - 3 9

SAMPLE

Matrix: solutions

HPLC V RI BLES

Colu mn: 250 X 4.6 Chirex 3022 (Phenomenex)

Mobile phase : Hexane: 1,2-dichloroethane: EtOH/trifluoroacetic acid 60 :35:5 (EtOH/

trifluoroacetic acid was premixed 20:1.)

Flow rate: 0.7-1

Injection volume: 20

D etec tor: UV 276

KEYWORDS

chiral; a = 1.08

REFERENCE

Cleveland, T. Pirkle-concept chiral stationary phases for the HPLC separation of pharmaceutical race-

mates .  J.Liq.Chromatogr. 1995, 18 6 4 9 - 6 7 1

S MPLE

Matrix: solutions

Sa mple p repa ra ti on : Inject a 20 |xL aliquot of a 1 mg/mL solution.

HPLCV RI BLES

Column: 250 X 4.6 10 ^m Chiralcel OD

M obile phase : Hexane: isopropanol: diethylamine 80:20:0.1

Flow rate: 0.5

Injection volume: 20

D etec tor: UV 275

CHROM TOGR M

Retention time: k' 0.69, 2.02 (enantiomers)

KEYWORDS

chiral

REFERENCE

Eke lund, J.; v an A rkens, A.; Bron num -Han sen, K.; Fich, K.; Olsen, L.; Pete r

 sen,

  RV. Chiral separations

of (3-blocking drug substances using chiral stationary phases. J.Chromatogr.A 1995,  708 2 5 3 - 2 6 1

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S MPLE

Matrix:  solutions

Sample preparat ion:

  Inject an aliquot of a 200

  |JLM

  solution in MeOH.

HPLCV RI BLES

Column:

  100 X 4.7 7 Lim Hypercarb (Shandon)

Mobile phase:  MeOH containing 5 mM N-benzyloxycarbonylglycyl-L-proline and 4.5 mM

NaOH

Colum n tem pera ture: 17

Inject ion vo lum e:  20

Detector: UV  270

CHROM TOGR M

Retent ion t ime:

  k' 18 (first enantiomer)

KEYWORDS

chiral; a = 1.09

REFERENCE

Huynh, N.-H.; Karlsson, A.; Pettersson, C. Enantiomeric separation of basic drugs using N-benzyloxy-

carbonylglyclyl-L-proline as counter ion in methanol. J.Chromatogr.A 1995,  705 2 7 5 - 2 8 7

SAMPLE

Matrix:

  solutions

HPLCV RI BLES

Column:  150 X 4.6 12 |xm l-myristoyl-2-[(13 -carboxyl)-tridecoyl]-sn-3-g lycerophosphocho-

line chemically bonded to silica (Regis)

Mobile phase:  M eCN : 100 mM pH 7.0 phos pha te buffer 20 :80

Flow rate: 1

De tector : UV 254

CHROMATOGRAM

R ete ntio n t ime : k 2.72

OTHER SUBST NCES

Also analyzed:

  acebutolol, alprenolol, antazo line, atenolol, betaxolol, bisoprolol, bopindolol,

bupranolol, carteolol, celiprolol, chloropyramine, chlorpheniramine, cicloprolol, cimeti-

dine, cinnarizine, cirazoline, clonidine, dilevalol, dimethindene, diphenhydramine, doxa-

zosin, esmolol, famotidine, isothipendyl, ketotifen, metiamide, moxonidine, nadolol, na-

phazoline, nifenalol, nizatidine, oxprenolol, pheniramine, phentolamine, pindolol,

pizotyline (pizotifen), practolol, prazosin, promethazine, propranolol, pyrilamine (mepyr-

amine), ranitidine, roxatidine, sotalol, tiamenidine, timolol, tramazoline, tripelennamine,

triprolidine, tymazoline, UK-14,304

REFERENCE

Kaliszan, R.; Nasal, A.; Turowski, M. Binding site for basic drugs on  a

r

acid  glycoprotein as revealed by

chemometric analysis of biochromatographic data. B iomed.Chromatogr. 1995, 9 211—215

SAMPLE

Matrix:  solutions

HPLC V RI BLES

Column:

  250 X 4.6 5 fjim Supelcosil LC-DP (A) or 250 X 4 5 p,m LiChrospher 100 RP-8 (B)

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Mobile phase:  M eCN : 0.025% phosph oric acid .buffer 2 5 :1 0 :5 (A) or 60 :2 5: 15 (B) (Buffer

was 9 mL concentrated phosphoric acid and 10 mL triethy lam ine in 900 mL water, adjust

pH to 3.4 with dilute phosphoric acid, make up to 1 L.)

Flow rate: 0.6

Inject ion vo lum e:

  25

D etecto r: UV 229

CHROM TOGR M

Retention time: 7.12 (A), 4.19 (B)

OTHER SUBST NCES

Also analyzed:  acebutolol, acepromazine, acetaminophen, acetazolamide, acetophenazine,

albuterol, alprazolam, amitriptyline, amobarbital, amoxapine, antipyrine, atenolol, atro-

pine,

  azatadine, baclofen, benzocaine, bromocriptine, brompheniramine, brotizolam,

bupivacaine, buspirone, butabarbital, butalbital, caffeine, carbamazepine, cetirizine,

chlorcyclizine, chlordiazepoxide, chlormezanone, chloroquine, chlorpheniramine,

chlorpromazine, chlorpropamide, chlorprothixene, chlorthalidone, chlorzoxazone, cimeti-

dine,

  cisapride, clomipramine, clonazepam, clonidine, clozapine, cocaine, codeine, colchi-

cine,  cyclizine, cyclobenzaprine, dantrolene, desipramine, diazepam, diclofenac, diflunisal,

diltiazem, diphenhydramine, diphenidol, diphenoxylate, dipyridamole, disopyramide, do-

butamine, doxapram, doxepin, droperidol, encainide, ethidium bromide, ethopropazine,

fenoprofen, fentanyl, flavoxate, fluoxetine, fluphenazine, flurazepam, flurbiprofen, fluvox-

amine, furosemide, glutethimide, glyburide, guaifenesin, haloperidol, homatropine, hy-

dralazin e, hyd rochlorothiazide, hydrocodone, hydromorphone, hydroxychloroquine, hydro-

xyzine, ibuprofen, imipramine, indomethacin, ketoconazole, ketoprofen, ketorolac,

labetalol, levorphanol, lidocaine, loratadine, lorazepam, lovastatin, loxapine, mazindol,

mefenamic acid, meperidine, mephenytoin, mepivacaine, mesoridazine, metaproterenol,

metformin, methadone, methdilazine, methocarbamol, methotrexate, methotrimeprazine,

methoxamine, methyldopa, methylphenidate, metoclopramide, metolazone, metronida-

zole,  midazolam, moclobemide, morphine, nadolol, nalbuphine, naloxone, naphazoline,

naproxen , nifedipine, nizatidin e, no repinep hrine, nortripty line, oxazepam, oxycodone, ox-

ymetazoline, paroxetine, pemoline, pentazocine, pentobarbital, pentoxifylline, perphena-

zine,

  pheniramine, phenobarbital, phenol, phenolphthalein, phentolamine, phenylbuta-

zone, phenyltoloxamine, phenytoin, pimozide, pindolol, piroxicam, pramoxine, prazepam,

prazosin, probenecid, procainamide, procaine, prochlorperazine, procyclidine, promazine,

promethazine, propafenone, propantheline, propiomazine, propofol, propranolol, protrip-

tyline, quazepam, quinidine, quinine, racemethorphan, ranitidine, remoxipride, risperi-

done, salicylic acid, scopolamine, secobarbital, sertraline, sotalol, spironolactone, sulfin-

pyrazone, sulindac, temazepam, terbutaline, terfenadine, tetracaine, theophylline,

thiethylperazine, thiopental, thioridazine, thiothixene, timolol, tocainide, tolbutamide,

tolmetin, trazodone, triamterene, triazolam, trifluoperazine, triflupromazine, trimepra-

zine,  trimethoprim, trimipramine, verapamil, warfarin, xylometazoline, yohimbine,

zopiclone

KEY WORDS

some details of plasma extraction

REFERENCE

Koves, E.M. Use of high-performance liquid chromatography-diode array detection in forensic toxicology.

J.ChromatogrA 1995, 692 103-119

SAMPLE

Matrix:  solutions

HPLCV RI BLES

Column:

  150 X 4.6 cellulose 3,5-dimethylphen ylcarbamate/10-und ecenoate bonded to

allylsilica

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Mobile phase:  Heptane: isopropanol: diethylamine 80:20:0.1

Flow rate: 1

Injection volume:  1000

Detector: UV 254

CHROMATOGRAM

Retention time:

  k' 1.61

KEYWORDS

chiral; a = 1.24

REFERENCE

Oliveros,  L.;  Lopez,  P.; M inguillon,  C;  Franco,  P.  Chiral chromatographic discrimination ability  of a

cellulose 3,5-dimethylphenylcarbamate/10-undecenoate mixed derivative fixed on  several chromato-

graphic matrices.  J.Liq.Chromatogr.

1995

18, 1521-1532

SAMPLE

Matrix:

  solutions

HPLCV RI BLES

Column:

  300 X 3.9 5 |xm Nova-Pak C18

Mobile phase:

  MeOH: buffer 30:70 (Buffer was pH 4.0 phosphate buffer (ionic strength =

0.1) containing 2.86 mM N, N-dimethyloctylamine, pH readjusted to 4.00 with 85 phos-

phoric acid.)

Column temperature: 30

Flow rate: 1

Injection volume:  100

Detector: UV 220

CHROMATOGRAM

Retention time: k

;

  2.81

OTHER SUBST NCES

Also analyzed:

  acebutolol, bunitrolol, carazolol, celiprolol, esmolol, mepindolol, timolol

REFERENCE

Hamoir, T.; Verlinden, Y.; Massart , D.L. Reversed-phase liquid chromatography of (3-adrenergic block ing

drugs in the presence of a  tailing suppressor.  J.Chromatogr.Sci.

1994

32 14-20

SAMPLE

Matrix:  solutions

HPLCV RI BLES

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-

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 temperature: 30

Flow rate: 2

Detector: UV 210

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OTHER SUBST NCES

Also analyzed:

  acepromazine, acetaminophen, acetophenazine, albuterol, aminophylline,

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

bital, aspirin, atenolol, atropin e, averme ctin, bar bital, benzo caine, 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, dextropropoxyphene, diamorphine, diazepam, diclofenac, diethylpropion,

diethylstilbestrol, diflunisal, digitoxin, digoxin, diltiazem, diphenhydramine, diphenoxy-

late,  diprenorphine, dipyrone, disulfiram, dopamine, doxapram, doxepin, dronabinol,

ephedrine, epinephrine, epinine, estradiol, estriol, estrone, ethacrynic acid, ethosuximide,

etonitazene, etorphine, eugenol, famotidine, fenbendazole, fencamfamine, fenoprofen, fen-

proporex, fentanyl, flubendazole, flufenamic acid, flunitrazepam, 5-fluorouracil, fluo-

xymesterone, fluphenazine, furosemide, gentisic acid, gitoxigenin, glipizide, glunixin,

glutethimide, glybenclamide, guaiacol, halazepam, haloperidol, hydrochlorothiazide,

hydrocodone, hydrocortisone, hydromorphone, hydroxyquinoline, ibogaine, ibuprofen, im-

inostilbene, imipramine, indomethacin, isocarbostyril, isocarboxazid, isoniazid, isoproter-

enol, isoxsuprine, ivermectin, ketamine, ketoprofen, kynurenic acid, levorphanol, Ii-

docaine, lorazepam, lormetazepam, loxapine, mazindol, mebendazole, meclizine,

meclofenamic acid, medazepam, mefenamic acid, megestrol, mepacrine, meperidine, me-

phentermine, mephenytoin, mephesin, mephobarbital, mepivacaine, mescaline, mesori-

dazine, methadone, methamphetamine, methapyrilene, methaqualone, methazolamide,

methocarbamol, methoxamine, methsuximide, methyl salicylate, methyldopa, methyldo-

pamine, methylphenidate, methylprednisolone, methyltestosterone, methyprylon, mibol-

erone, morphine, nadolol, nalorphine, naloxone, naltrexone, naphazoline, naproxen, ne-

fopam, niacinamide, nicotine, nicotinic acid, nifedipine, niflumic acid, nitrazepam,

norepinephrine, nortriptyline, noscapine, nylidrin, oxazepam, oxycodone, oxymorphone,

oxyphenbutazone, oxytetracycline, papaverine, pargyline, pemoline, pentazocine, pento-

barbital, persantine, phenacetin, phenazocine, phenazopyridine, phencyclidine, phendi-

metrazine, phenelzine, pheniramine, phenobarbital, phenothiazine, phensuximide, phen-

termine, phenylbutazone, phenylephrine, phenylpropanolamine, piperocaine, prazepam,

prednisolone, primidon e, probenecid, prog esterone, propiomazine, propranolol, propylpar-

aben, pseudoephedrine, puromycin, pyrilamine, pyrithyldione, quazepam, quinaldic acid,

quinidine, quinine, ranitidine, recinnamine, reserpine, resorcinol, saccharin, albuterol,

salicylamide, salicylic acid, scopolamine, scopoletin, secobarbital, strychnine, sulfacetam-

ide,  sufadiazine, sulfadimethoxine, sulfaethidole, sulfamerazine, sulfamethazine, sulfa-

methoxizole, sulfanilamide, sulfapyridine, sulfasoxizole, sulindac, tamoxifen, temazepam,

testosterone, tetracaine, tetracycline, tetramisole, thebaine, theobromine, theophylline,

thiabendazole, thiamine, thiamylal, thiobarbituric acid, thioridazine, thiosalicylic acid,

thiothixene, thymol, tolazamide, tolazoline, tobutamide, tolmetin, tranylcypromine, tri-

amcinolone, tribenzylamine, trichloromethiazide, trifluoperazine, trihexyphenidyl, tri-

methoprim, tripelennamine, triprolidine, tropacocaine, tyramine, verapamil, vincamine,

warfarin, yohimbine, zoxazolamine

REFERENCE

Hill, D.W.; Kind, A.J. Reversed-phase solvent grad ient HPLC reten tion indexes of drugs.   J.Anal.ToxicoL

1994,  18 233-242

SAMPLE

Matrix:

  solutions

HPLCV RI BLES