GAS CHROMATOGRAPHY OF BARBITURATES PHENOLIC ALKALOIDS AND XANTHINE BASES - FLASH-HEATER METHYLATION BY MEANS OF TRIMETHYLANILINIUM HYDROXIDE

被引：210

作者：

BROCHMAN.E

OKE, TO

机构：

[1] Department of Pharmaceutical Chemistry, University of California School of Pharmacy, San Francisco, California

[2] Chas Pfizer & Co., Inc, Brooklyn, New York

来源：

JOURNAL OF PHARMACEUTICAL SCIENCES | 1969年 / 58卷 / 03期

关键词：

Barbiturates—analysis; GLC—analysis; Methylation—gas chromatograph flash heater; NMR spectroscopy—structure; Phenolic alkaloids—analysis; Trimethylanilium hydroxide—methylating agent; xanthine bases—analysis;

D O I：

10.1002/jps.2600580322

中图分类号：

R914 [药物化学];

学科分类号：

100701 ;

摘要：

Injection of methanol solutions of trimethylanilinium salts of barbiturates, phenolic alkaloids, and dimethylxanthines produced thermal decomposition in the injection port to give methyl derivatives suitable for quantitative gas chromatography. Trimethylanilinium hydroxide appeared to be superior to tetramethylammonium hydroxide for instantaneous methylation of these compounds. Quantitative methylation was achieved under a variety of experimental conditions. The change in retention time resulting from methylation may be used for identification purposes. The 1,3‐dimethyl structure of methylated barbiturates was confirmed by NMR spectroscopy. Copyright © 1969 Wiley‐Liss, Inc., A Wiley Company

引用

页码：370 / &

共 12 条

[1] SEPARATION AND IDENTIFICATION OF BARBITURATES AND SOME RELATED COMPOUNDS BY MEANS OF GAS-LIQUID CHROMATOGRAPHY [J].

BROCHMANNHANSSE.E ;

SVENDSEN, AB .

JOURNAL OF PHARMACEUTICAL SCIENCES, 1962, 51 (04) :318-&

[2]

BROCHMANNHANSSE.E, 1968, THEORY APPLICATIONS, P182

[3] GAS CHROMATOGRAPHY AND ITS APPLICATION TO PHARMACEUTICAL ANALYSIS [J].

BROCHMANNHANSSEN, E .

JOURNAL OF PHARMACEUTICAL SCIENCES, 1962, 51 (11) :1017-&

[4]

COOK JG, 1961, J CHROMATOGR, V6, P182

[5]

GUDZINOWICZ BJ, 1967, GAS CHROMATOGRAPHIC, P183

[6]

KROMAN HS, 1968, THEORY APPLICATIO ED, P182

[7] GAS CHROMATOGRAPHIC IDENTIFICATION AND DETERMINATION OF BARBITURATES [J].

MARTIN, HF ;

DRISCOLL, JL .

ANALYTICAL CHEMISTRY, 1966, 38 (02) :345-&

[8]

MCGEE J, 1966, ANAL BIOCHEM, V14, P305

[9] PREPARATION OF METHYL ESTERS FOR GAS LIQUID CHROMATOGRAPHY OF ACIDS BY PYROLYSIS OF TETRAMETHYLAMMONIUM SALTS [J].

ROBB, EW ;

WESTBROO.JJ .

ANALYTICAL CHEMISTRY, 1963, 35 (11) :1644-&

[10] ON-COLUMN METHYLATION OF BARBITURIC ACIDS [J].

STEVENSON, GW .

ANALYTICAL CHEMISTRY, 1966, 38 (13) :1948-+

← 1 2 →