Simple and sensitive analysis of nereistoxin and its metabolites in human serum using headspace solid-phase microextraction and gas chromatography mass spectrometry

被引:30
作者
Namera, A
Watanabe, T
Yashiki, M
Kojima, T
Urabe, T
机构
[1] Hiroshima Univ, Sch Med, Dept Legal Med, Minami Ku, Hiroshima 7348551, Japan
[2] Sera Cent Hosp, Hiroshima 7221112, Japan
关键词
D O I
10.1093/chromsci/37.3.77
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
A simple method for the analysis of nereistoxin and its metabolites in human serum using headspace solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) is developed. A vial containing a serum sample, 5M sodium hydroxide, and benzylacetone (internal standard) is heated to 70°C, and an SPME fiber is exposed for 30 min in the headspace of the vial. The compounds extracted by the fiber are desorbed by exposing the fiber in the injection port of the GC-MS. The calibration curves show linearity in the range of 0.05-5.0 μg/mL for nereistoxin and N-methyl-N-(2-methylthio-1-methylthiomethyl)ethylamine, 0.01-5.0 μg/mL for S,S-dimethyl dihydronereistoxin, and 0.5-10 μg/mL for 2-methylthio-1-methylthiomethylethylamine in serum. No interferences are found, and the analysis time is 50 min for one sample. In addition, this proposed method is applied to a patient who attempted suicide by ingesting Padan 4R, a herbicide. Padan 4R contains 4% cartap hydrochloride, which is an analogue of nereistoxin. Nereistoxin and its metabolites are detected in the serum samples collected from the patient during hospitalization. The concentration ranges of nereistoxin in the serum are 0.09-2.69 μg/mL.
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页码:77 / 82
页数:6
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