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Gas chromatographic/mass spectrometric identification and quantification of aniline after extraction from serum and derivatization with 4-carbethoxyhexafluorobutyryl chloride, a new derivative.
Ther Drug Monit. 1999 Apr; 21(2):238-42.TD

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 microL of 4-carbethoxyhexafluorobutyryl chloride. After evaporating the excess derivatizing reagent, the residue was reconstituted in 50 microL of ethyl acetate and injected into the GC/MS. A positive identification of derivatized aniline can be made from the strong molecular ion 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.

Authors+Show Affiliations

Department of Pathology and Laboratory Medicine, University of Texas-Houston Health Science Center, 77030, USA.No affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

10217346

Citation

Dasgupta, A, and C Jagannath. "Gas Chromatographic/mass Spectrometric Identification and Quantification of Aniline After Extraction From Serum and Derivatization With 4-carbethoxyhexafluorobutyryl Chloride, a New Derivative." Therapeutic Drug Monitoring, vol. 21, no. 2, 1999, pp. 238-42.
Dasgupta A, Jagannath C. Gas chromatographic/mass spectrometric identification and quantification of aniline after extraction from serum and derivatization with 4-carbethoxyhexafluorobutyryl chloride, a new derivative. Ther Drug Monit. 1999;21(2):238-42.
Dasgupta, A., & Jagannath, C. (1999). Gas chromatographic/mass spectrometric identification and quantification of aniline after extraction from serum and derivatization with 4-carbethoxyhexafluorobutyryl chloride, a new derivative. Therapeutic Drug Monitoring, 21(2), 238-42.
Dasgupta A, Jagannath C. Gas Chromatographic/mass Spectrometric Identification and Quantification of Aniline After Extraction From Serum and Derivatization With 4-carbethoxyhexafluorobutyryl Chloride, a New Derivative. Ther Drug Monit. 1999;21(2):238-42. PubMed PMID: 10217346.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Gas chromatographic/mass spectrometric identification and quantification of aniline after extraction from serum and derivatization with 4-carbethoxyhexafluorobutyryl chloride, a new derivative. AU - Dasgupta,A, AU - Jagannath,C, PY - 1999/4/27/pubmed PY - 1999/4/27/medline PY - 1999/4/27/entrez SP - 238 EP - 42 JF - Therapeutic drug monitoring JO - Ther Drug Monit VL - 21 IS - 2 N2 - 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 microL of 4-carbethoxyhexafluorobutyryl chloride. After evaporating the excess derivatizing reagent, the residue was reconstituted in 50 microL of ethyl acetate and injected into the GC/MS. A positive identification of derivatized aniline can be made from the strong molecular ion 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. SN - 0163-4356 UR - https://www.unboundmedicine.com/medline/citation/10217346/Gas_chromatographic/mass_spectrometric_identification_and_quantification_of_aniline_after_extraction_from_serum_and_derivatization_with_4_carbethoxyhexafluorobutyryl_chloride_a_new_derivative_ L2 - http://dx.doi.org/10.1097/00007691-199904000-00016 DB - PRIME DP - Unbound Medicine ER -