Merck
  • Home
  • Search Results
  • A new silylating reagent - dimethyl(3,3,3-trifluoropropyl)silyldiethylamine - for the derivatisation of non-steroidal anti-inflammatory drugs prior to gas chromatography-mass spectrometry analysis.

A new silylating reagent - dimethyl(3,3,3-trifluoropropyl)silyldiethylamine - for the derivatisation of non-steroidal anti-inflammatory drugs prior to gas chromatography-mass spectrometry analysis.

Journal of chromatography. A (2014-05-13)
Magda Caban, Katarzyna Mioduszewska, Paulina Lukaszewicz, Natalia Migowska, Piotr Stepnowski, Marek Kwiatkowski, Jolanta Kumirska
ABSTRACT

This paper discusses a new silylating reagent - dimethyl(3,3,3-trifluoropropyl)silyldiethylamine (DIMETRIS) - for the derivatisation of non-steroidal anti-inflammatory drugs (NSAIDs) prior to GC-MS analysis. DIMETRIS reacts with seven target compounds (diclofenac, ibuprofen, ketoprofen, naproxen, flurbiprofen and paracetamol, as well as salicylic acid, a degradation product of acetylsalicylic acid) at 30°C for 30min, producing mono-O-dimethyltrifluoropropylsilyl (mono-O-DMTFPS) derivatives. The mass spectra of these new derivatives are given and fully interpreted. The usefulness of mono-O-DMTFPS derivatives for the qualitative and quantitative analysis of NSAIDs using GC-MS is compared with that of trimethylsilyl and methyl analogues. Methyl derivatives are found to be less appropriate for this purpose because they yield the lowest detector responses during GC-MS measurements. Both silyl derivatives are more suitable for determining such NSAIDs, although the matrix effect with mono-O-DMTFPS derivatives is smaller. Finally, SPE-GC-MS(SIM) based on the derivatisation of NSAIDs by DIMETRIS is evaluated, validated and applied to the determination of these drugs in sea water (Baltic Sea) and wastewater samples collected in Poland. This work confirms that DIMETRIS is suitable for the trace analysis of NSAIDs in real samples and provides an interesting alternative to silylating and methylating reagents.

MATERIALS
Product Number
Brand
Product Description

Supelco
Salicylic acid, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Salicylic acid, certified reference material, TraceCERT®
Sigma-Aldrich
Salicylic acid, BioXtra, ≥99.0%
Sigma-Aldrich
Salicylic acid, suitable for plant cell culture
Supelco
N,O-Bis(trimethylsilyl)trifluoroacetamide with trimethylchlorosilane, with 1% trimethylchlorosilane, for GC derivatization, LiChropur
Sigma-Aldrich
Salicylic acid, ReagentPlus®, ≥99%
Sigma-Aldrich
Chlorotrimethylsilane, purified by redistillation, ≥99%
Sigma-Aldrich
Chlorotrimethylsilane, ≥98.0% (GC)
Sigma-Aldrich
Chlorotrimethylsilane, puriss., ≥99.0% (GC)
Supelco
N,O-Bis(trimethylsilyl)trifluoroacetamide with trimethylchlorosilane, for GC derivatization, LiChropur, contains 1% TMCS, 99% (excluding TMCS)
Sigma-Aldrich
Chlorotrimethylsilane, produced by Wacker Chemie AG, Burghausen, Germany, ≥99.0% (GC)
Sigma-Aldrich
2-Methylanthracene, 97%
Sigma-Aldrich
Salicylic acid, ACS reagent, ≥99.0%
Sigma-Aldrich
4-Dimethylaminoantipyrine, reactive nitrogen species scavenger
Sigma-Aldrich
Acetylsalicylic acid, analytical standard
Sigma-Aldrich
Acetylsalicylic acid, ≥99.0%
Sigma-Aldrich
Salicylic acid, puriss. p.a., ≥99.0% (T)
Supelco
N,O-Bis(trimethylsilyl)trifluoroacetamide with trimethylchlorosilane, for GC derivatization, LiChropur, contains 10% TMCS, 98% (excluding TMCS)
Sigma-Aldrich
Salicylic acid, meets analytical specification of Ph. Eur., BP, USP, 99.5-100.5% (calc. to the dried substance)
Sigma-Aldrich
Salicylic acid, ≥99%, FG
USP
Salicylic acid, United States Pharmacopeia (USP) Reference Standard
Salicylic acid, European Pharmacopoeia (EP) Reference Standard
Supelco
Salicylic acid, 1.0 mg/mL in acetonitrile, ampule of 1 mL, certified reference material, Cerilliant®
Paracetamol, European Pharmacopoeia (EP) Reference Standard
Supelco
Chlorotrimethylsilane, for GC derivatization, LiChropur, ≥99.0% (GC)
Acetylsalicylic acid, European Pharmacopoeia (EP) Reference Standard
Acetylsalicylic acid for peak identification, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Acetaminophen, analytical standard
Sigma-Aldrich
Acetaminophen, BioXtra, ≥99.0%
Sigma-Aldrich
Acetaminophen, meets USP testing specifications, 98.0-102.0%, powder