Simultaneous determination of five hypertoxic rodenticides in serum by gas chromatography-mass spectrometry

doi:10.3724/SP.J.1123.2014.11024

Abstract

Abstract:

A fast analytical method based on gas chromatography-mass spectrometry (GC-MS) was established for the simultaneous determination of tetramine, fluoroacetamide, sodium fluoroacetate, gliftor Ⅰ and gliftor Ⅱ in serum. At pH 2.0, sodium fluoroacetate was derivatizated at room temperature for 5 min by using N,N-diethyl-p-phenylenediamine as the derivatization reagent and N,N'-dicyclohexylcarbodiimide as the catalyst. The derivative and other rodenticides were extracted with ethyl acetate and concentrated with nitrogen at 50 ℃, then determined by GC-MS in selected ion monitoring (SIM) mode, and quantified with matrix-match standard solutions. The analysis was carried out on an ionic liquid chromatographic capillary column (SLB-IL59, 30 m×0.25 mm×0.20 μm, maximum temperature 300 ℃) at a flow rate of 1.0 mL/min, and the five rodenticides were successfully separated in 15 min when temperature programming was used. The results showed that the calibration curves were linear in the range of 0.01-1.0 mg/L, except for fluoroacetamide (0.02-2.0 mg/L) and tetramine (0.02-10 mg/L), with correlation coefficients (R²) greater than 0.995, and the limits of detection (LODs) were 0.001-0.002 mg/L (S/N=3). The recoveries were 84.0%-110.0% at three different spiked levels, and the relative standard deviations (RSDs) were 2.9%-7.5%(n=6). The method is simple, accurate, highly sensitive and suitable for the detection of the five hypertoxic rodenticides in serum for toxicological purposes.

Key words: gas chromatography-mass spectrometry (GC-MS), hypertoxic rodenticide, serum

CLC Number:

O658

HUANG Huiqiu, HUANG Xun, YU Jingsun. Simultaneous determination of five hypertoxic rodenticides in serum by gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, 2015, 33(3): 323-328.

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