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, Amitava
AU - Jagannath, Chinnaswamy
PY - 1999/4/1
Y1 - 1999/4/1
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 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.
AB - 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.
KW - 4-carbethoxyhexafluorobutyryl
KW - Aniline
KW - Gas chromatography-Mass spectrometry
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U2 - 10.1097/00007691-199904000-00016
DO - 10.1097/00007691-199904000-00016
M3 - Article
C2 - 10217346
AN - SCOPUS:0032923414
SN - 0163-4356
VL - 21
SP - 238
EP - 242
JO - Therapeutic Drug Monitoring
JF - Therapeutic Drug Monitoring
IS - 2
ER -