分散固相萃取-超高效液相色谱-串联质谱法测定禽蛋中氟虫腈及其代谢产物

doi:10.3724/SP.J.1123.2017.08018

摘要/Abstract

摘要：

建立了分散固相萃取-超高效液相色谱-串联质谱检测禽蛋中氟虫腈及其代谢产物氟甲腈、氟虫腈硫醚和氟虫腈砜的方法。样品用含1%（体积分数）乙酸的乙腈提取后，加无水硫酸钠、十八烷基键合硅胶（C₁₈-N）及氨基-丙基乙二胺（NH₂-PSA）3种净化剂，旋涡振荡，对样品进行净化。以Shim-pack GIST C₁₈色谱柱（50 mm×2.1 mm，2 μm）进行分离，以甲醇和1 mmol/L乙酸铵水溶液为流动相进行梯度洗脱，在电喷雾离子源负离子模式和多反应检测（MRM）模式下进行定性定量分析。考察了净化剂中无水硫酸钠、C₁₈-N和NH₂-PSA的用量对加标回收率的影响，优化了实验条件。结果表明：4种化合物在0.4~100 μg/L范围内线性关系良好，相关系数r² ≥ 0.9989；回收率为95.09%~103.26%；定量限为0.2 μg/kg。该方法前处理简单，回收率高，重复性好，可作为禽蛋中氟虫腈及其代谢产物的有效检测方法。

关键词: 超高效液相色谱-串联质谱, 分散固相萃取, 氟虫腈, 禽蛋

Abstract:

An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed to determine fipronil and its metabolites (fipronil desulfinyl, fipronil sulfone and fipronil sulfide) in bird eggs. The samples were extracted with acetonitrile containing 0.1%(v/v) acetic acid, and then purified by a mixture of anhydrous sodium sulfate, octadecyl carbon silica gel (C₁₈-N) sorbent and ethylenediamine-N-propyl carbon silica gel (NH₂-PSA) sorbent. The analysis was performed by a UPLC-MS/MS system with Shim-pack GIST C₁₈ column (50 mm×2.1 mm, 2 μm). The mobile phases consisted of methanol and 1 mmol/L ammonium acetate aqueous solution by gradient elution, and multiple reaction monitoring (MRM) mode with negative electrospray ionization was used. The effect of the dosages of anhydrous sodium sulfate, C₁₈-N and NH₂-PSA in cleaning-up agent was studied. The main influence factors and analytical conditions were modified. Four linear calibration curves were obtained with correlation coefficients r² ≥ 0.9989. The recoveries were determined at three concentrations and ranged from 95.09%-103.26%. The limit of quantification (LOQ) was 0.2 μg/kg. It is suitable for the determination of fipronil and its metabolites in bird eggs.

Key words: bird eggs, dispersive solid phase extraction, fipronil, ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

中图分类号:

O658

励炯, 郑锌, 王红青, 邱红钰. 分散固相萃取-超高效液相色谱-串联质谱法测定禽蛋中氟虫腈及其代谢产物[J]. 色谱, 2017, 35(12): 1211-1215.

LI Jiong, ZHENG Xin, WANG Hongqing, QIU Hongyu. Determination of fipronil and its metabolites in bird eggs by ultra-performance liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction[J]. Chinese Journal of Chromatography, 2017, 35(12): 1211-1215.

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