Enhancement of chemical derivatization of steroids by gas chromatography/mass spectrometry (GC/MS)

被引：48

作者：

Bowden, John A. ^{[1
]}

Colosi, Dominic M. ^{[1
]}

Mora-Montero, Diana C. ^{[1
]}

Garrett, Timothy J. ^{[2
]}

Yost, Richard A. ^{[1
]}

机构：

[1] Univ Florida, Dept Chem, Gainesville, FL 32611 USA

[2] Univ Florida, Dept Med, Biomed Mass Spectrometry Lab, Gainesville, FL 32610 USA

来源：

JOURNAL OF CHROMATOGRAPHY B-ANALYTICAL TECHNOLOGIES IN THE BIOMEDICAL AND LIFE SCIENCES | 2009年 / 877卷 / 27期

关键词：

Chemical derivatization; Derivatization enhancement; Gas chromatography/mass spectrometry; Microwave-accelerated derivatization; Silylation; Steroid profiling; Steroids; SOLID-PHASE EXTRACTION; ENDOCRINE DISRUPTING COMPOUNDS; MASS-SPECTROMETRY; TRIMETHYLSILYL DERIVATIZATION; WATER; SILYLATION; ESTROGENS; HORMONES; ESTRONE; 17-ALPHA-ETHINYLESTRADIOL;

D O I：

10.1016/j.jchromb.2009.08.005

中图分类号：

Q5 [生物化学];

学科分类号：

071010 ; 081704 ;

摘要：

Steroid derivatization was investigated by varying the experimental parameters (reagent, reaction time, and reaction temperature) to determine the optimal conditions for individual steroids, and for larger subsets. Three methods of derivatization enhancement were also investigated: the use of sonication, the use of a microwave heating, and the addition of solvents to the reaction mixture. On a comprehensive level, derivatization using N-methyl-N-trintethylsilyl-trifluoroacetamide (MSTFA) was most efficient, while the application of solvent addition and microwave heating, in several cases, provided a clear enhancement. In addition, generalized rules for steroid derivatization are described. (C) 2009 Elsevier B.V. All rights reserved.

引用

页码：3237 / 3242

页数：6

共 30 条

[1] AN IMPROVED METHOD FOR STEROID PROFILE ANALYSIS USING CAPILLARY GAS-CHROMATOGRAPHY
ADATIA, R
COOKE, M
[J]. CHROMATOGRAPHIA, 1988, 25 (07) : 598 - 602
[2] Agatha G., 1999, CLIN LAB, V45, P387
[3] Determination of endogenous and synthetic glucocorticoids in human urine by gas chromatography-mass spectrometry following microwave-assisted derivatization
Amendola, L
Garribba, F
Botrè, F
[J]. ANALYTICA CHIMICA ACTA, 2003, 489 (02) : 233 - 243
[4] Evaluation of Derivatization Strategies for the Comprehensive Analysis of Endocrine Disrupting Compounds using GC/MS
Bowden, John A.
Colosi, Dominic M.
Mora-Montero, Diana C.
Garrett, Timothy J.
Yost, Richard A.
[J]. JOURNAL OF CHROMATOGRAPHIC SCIENCE, 2009, 47 (01) : 44 - 51
[5] Analysis of hormonal steroids in fish plasma and bile by coupling solid-phase extraction to GC/MS
Budzinski, H.
Devier, M. H.
Labadie, P.
Togola, A.
[J]. ANALYTICAL AND BIOANALYTICAL CHEMISTRY, 2006, 386 (05) : 1429 - 1439
[6] Diagnosis of congenital adrenal hyperplasia by rapid determination of 17α-hydroxyprogesterone in dried blood spots by gas chromatography/mass spectrometry following microwave-assisted silylation
Deng, CH
Ji, J
Zhang, LJ
Zhang, XM
[J]. RAPID COMMUNICATIONS IN MASS SPECTROMETRY, 2005, 19 (20) : 2974 - 2978
[7] An assessment of estrogenic organic contaminants in Canadian wastewaters
Fernandez, Marc P.
Ikonomou, Michael G.
Buchanan, Ian
[J]. SCIENCE OF THE TOTAL ENVIRONMENT, 2007, 373 (01) : 250 - 269
[8] Extending the breadth of metabolite profiling by gas chromatography coupled to mass spectrometry
Fiehn, Oliver
[J]. TRAC-TRENDS IN ANALYTICAL CHEMISTRY, 2008, 27 (03) : 261 - 269
[9] USE OF DIFFERENT SILYLATING AGENTS FOR STRUCTURE ANALYSES OF STEROIDS
GLEISPACH, H
[J]. JOURNAL OF CHROMATOGRAPHY, 1974, 91 (APR24): : 407 - 412
[10] Halket JM., 1993, HDB DERIVATIVES CHRO

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