Direct silylation of Trypanosoma brucei metabolites in aqueous samples and their GC-MS/MS analysis.

Direct silylation of Trypanosoma brucei metabolites in aqueous samples and their GC-MS/MS analysis.

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences (2014-08-05)

Peter Podolec, Alexandra Hengerics Szabó, Jaroslav Blaško, Róbert Kubinec, Renáta Górová, Jozef Višňovský, Anna Gnipová, Anton Horváth, Václav Bierhanzl, Tomáš Hložek, Radomír Čabala

PMID25089958

ABSTRACT

A simple two-step method for the derivatization of polar compounds (lactate, alanine, glycerol, succinate and glucose) using hexamethyldisilazane (HMDS) and N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) was developed. This method allows direct derivatization of aqueous samples wihout sample pretreatment. The method was used for the analysis of the metabolites of the unicellular organism Trypanosoma brucei. The limits of detection by GC-MS/MS analysis were in the range of 0.02 mg L(-1) for glucose to 0.85 mg L(-1) for lactate.

MATERIALS

Product Number

Brand

Product Description

699640

Sigma-Aldrich

Carbon, mesoporous, less than 100 ppm Al, Ti, Fe, Ni, Cu, and Zn combined

PHR1320

Supelco

Residual Solvent - Acetonitrile(solution in DMSO), Pharmaceutical Secondary Standard; Certified Reference Material

A0325000

Alanine, European Pharmacopoeia (EP) Reference Standard

93067

Sigma-Aldrich

Activated Charcoal Norit^®, Norit^® SX2, powder, from peat, multi-purpose activated charcoal, steam activated and acid washed

15524

Sigma-Aldrich

Glycerol solution, puriss., meets analytical specification of Ph. Eur., BP, 84-88%

22874

Sigma-Aldrich

Activated Charcoal Norit^®, Norit^® PK 1-3, from peat, steam activated, granular

53663

Sigma-Aldrich

Activated Charcoal Norit^®, Norit^® SX ultra, from peat, steam activated and acid washed, highly purified, powder

T6381

Supelco

N,O-Bis(trimethylsilyl)trifluoroacetamide with trimethylchlorosilane, with 1% trimethylchlorosilane, derivatization grade (GC derivatization), LiChropur^™

PHR1020

Supelco

Glycerin, Pharmaceutical Secondary Standard; Certified Reference Material

PHR1215

Supelco

Lactic acid, Pharmaceutical Secondary Standard; Certified Reference Material

699624

Sigma-Aldrich

Carbon, mesoporous, nanopowder, graphitized, less than 250 ppm Al, Ti, Fe, Ni, Cu, and Zn combined

702102

Sigma-Aldrich

Carbon, mesoporous

15209

Supelco

N,O-Bis(trimethylsilyl)trifluoroacetamide with trimethylchlorosilane, derivatization grade (GC derivatization), LiChropur^™, contains 10% TMCS, 98% (excluding TMCS)

W261114

Sigma-Aldrich

Lactic acid, natural, ≥85%

W261106

Sigma-Aldrich

Lactic acid, 88%, FCC

L6661

Sigma-Aldrich

Lactic acid, meets USP testing specifications

49781

Sigma-Aldrich

Glycerol solution, 83.5-89.5% (T)