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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