Methods to reduce background interferences in electron-capture gas chromatographic analysis of valproic acid and its unsaturated metabolites after derivatization with pentafluorobenzyl bromide

被引：12

作者：

Dills, RL ^{[1
]}

Shen, DD ^{[1
]}

机构：

[1] UNIV WASHINGTON,SCH PHARM,DEPT PHARMACEUT,SEATTLE,WA 98195

来源：

JOURNAL OF CHROMATOGRAPHY B | 1997年 / 690卷 / 1-2期

关键词：

valproic acid; medium-chain fatty acids; fatty acids; pentafluorobenzyl bromide;

D O I：

10.1016/S0378-4347(96)00405-7

中图分类号：

Q5 [生物化学];

学科分类号：

071010 ; 081704 ;

摘要：

Analysis of the branched, medium-chain fatty acid anticonvulsant, valproic acid, and its unsaturated metabolites by gas chromatography with electron-capture detection suffered from background interference caused by the derivatizing reagent pentafluorobenzyl bromide. Background was reduced by keeping the derivatization anhydrous, using an inert solvent, minimizing the amount of pentafluorobenzyl bromide, using hypernucleophilic bases and displacing the derivatization solvent with isooctane. However, these strategies proved difficult to reproduce. Post-derivatization clean-up with HPLC was much more reliable and provided sufficient sensitivity for the analysis of extracts of plasma and brain homogenate. The assay was validated for plasma and brain samples from humans, rats and mice.

引用

页码：139 / 152

页数：14

共 47 条

[1] CAPILLARY GAS-CHROMATOGRAPHY MASS-SPECTROMETRY OF VALPROIC ACID METABOLITES IN SERUM AND URINE USING TERT-BUTYLDIMETHYLSILYL DERIVATIVES [J].

ABBOTT, FS ;

KASSAM, J ;

ACHEAMPONG, A ;

FERGUSON, S ;

PANESAR, S ;

BURTON, R ;

FARRELL, K ;

ORR, J .

JOURNAL OF CHROMATOGRAPHY, 1986, 375 (02) :285-298

[2] DISTRIBUTION OF UNSATURATED METABOLITES OF VALPROATE IN HUMAN AND RAT-BRAIN - PHARMACOLOGICAL RELEVANCE [J].

ADKISON, KDK ;

OJEMANN, GA ;

RAPPORT, RL ;

DILLS, RL ;

SHEN, DD .

EPILEPSIA, 1995, 36 (08) :772-782

[3] POLYFLUOROARENES .4. 2,3,4,5,6-PENTAFLUOROTOLUENE AND RELATED COMPOUNDS [J].

BIRCHALL, JM ;

HASZELDINE, RN .

JOURNAL OF THE CHEMICAL SOCIETY, 1961, (SEP) :3719-&

[4]

BLAU K, 1978, HDB DERIVATIVES CHRO, P108

[5] DESICCANT EFFICIENCY IN SOLVENT AND REAGENT DRYING .6. DRYING OF GROSSLY WET ETHER EXTRACTS [J].

BURFIELD, DR ;

SMITHERS, RH .

JOURNAL OF CHEMICAL EDUCATION, 1982, 59 (08) :703-704

[6] DETERMINATION OF ANTIEPILEPTIC DRUGS [J].

BURKE, JT ;

THENOT, JP .

JOURNAL OF CHROMATOGRAPHY, 1985, 340 (MAY) :199-241

[7]

CHAN SC, 1980, CLIN CHEM, V26, P1528

[8] DETERMINATION OF ACETYL AND FORMYL GROUPS AS PENTAFLUOROBENZYL ESTERS BY MEANS OF GAS-LIQUID-CHROMATOGRAPHY WITH ELECTRON-CAPTURE DETECTION [J].

CHAUHAN, J ;

DARBRE, A .

JOURNAL OF CHROMATOGRAPHY, 1982, 240 (01) :107-115

[9] IMPROVED PROCEDURE FOR PREPARATION OF PENTAFLUOROBENZYL DERIVATIVES OF CARBOXYLIC-ACIDS FOR ANALYSIS BY GAS-CHROMATOGRAPHY WITH ELECTRON-CAPTURE DETECTION [J].

DANESHVAR, MI ;

BROOKS, JB .

JOURNAL OF CHROMATOGRAPHY-BIOMEDICAL APPLICATIONS, 1988, 433 :248-256

[10] SENSITIVE CAPILLARY GAS-CHROMATOGRAPHIC MASS-SPECTROMETRIC METHOD FOR THE THERAPEUTIC DRUG-MONITORING OF VALPROIC ACID AND 7 OF ITS METABOLITES IN HUMAN SERUM - APPLICATION OF THE ASSAY FOR A GROUP OF PEDIATRIC EPILEPTICS [J].

DARIUS, J ;

MEYER, FP .

JOURNAL OF CHROMATOGRAPHY B-BIOMEDICAL APPLICATIONS, 1994, 656 (02) :343-351

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