Gas chromatographic/mass spectrometric identification and quantification of aniline after extraction from serum and derivatization with 4- carbethoxyhexafluorobutyryl chloride, a new derivative

Amitava Dasgupta, Chinnaswamy Jagannath

Research output: Contribution to journalArticle

4 Scopus citations

Abstract

Aniline, widely used as an intermediate in the synthesis of dye, is also used in the manufacture of pharmaceuticals, photographic developers, shoe polish, and other common substances. Exposure to aniline is toxic because it produces methemoglobin. Aniline levels are usually not measured in serum; in humans, blood methemoglobin levels are often measured as an index of exposure to aniline. In this article, we describe a method for the identification and the quantification of aniline by gas chromatography/mass spectrometry (GC/MS) after its extraction from human serum and derivatization with 4- carbethoxyhexafluorobutyryl chloride. Aniline, as well as the internal standard N-methyl aniline, was extracted from alkaline serum using chloroform. Aniline and the internal standard were derivatized with 50 μL of 4-carbethoxyhexafluorobutyryl chloride. After evaporating the excess derivatizing reagent, the residue was reconstituted in 50 μL of ethyl acetate and injected into the GC/MS. A at m/z 343. Similarly, derivatized internal standard showed a strong molecular ion at m/z 357. The within-run and between-run precisions of the assay were 3.8% and 5.8%, respectively, at an aniline concentration of 5 mg/L. The assay was linear for serum aniline concentrations of 0.5 mg/L to 25.0 mg/L. The detection limit was 0.1 mg/L. The assay was not affected by lipemia, hemolysis, or high bilirubin concentration in serum, and the assay was applicable to whole blood. We also fed mice (C57bl/6) with various concentrations of aniline and measured methemoglobin and blood concentrations of aniline. The methemoglobin percentage and aniline concentrations in blood increased with increasing aniline doses.

Original languageEnglish (US)
Pages (from-to)238-242
Number of pages5
JournalTherapeutic Drug Monitoring
Volume21
Issue number2
DOIs
StatePublished - Apr 1 1999

Keywords

  • 4-carbethoxyhexafluorobutyryl
  • Aniline
  • Gas chromatography-Mass spectrometry

ASJC Scopus subject areas

  • Pharmacology
  • Pharmacology (medical)

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