超高效液相色谱-串联质谱法快速分析氰霜唑及其代谢物 CCIM在水果中的残留

Rapid Analysis of Cyazofamid and CCIM Residues in Fruits by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry

摘要:

为评价氰霜唑及其主要代谢物4-氯-5-（4-甲苯基）-1H-咪唑-2-腈（CCIM）在水果中的安全性，建立了同时检测氰霜唑及其代谢物CCIM的高效液相色谱-串联质谱法。待测样品采用含体积分数1.0%乙酸的乙腈溶液提取，经十八烷基硅烷键合相（C₁₈）粉末和弗罗里硅土粉末净化后，以Capcell PAK C18色谱柱（150 mm×2.0 mm，5 μm）进行 UPLC分离，采用质谱多重反应监测模式（MRM）进行测定。结果表明，氰霜唑和CCIM在0.001~0.040 μg/mL时，质量浓度与峰面积呈良好的线性关系（R≥0.999 3），在0.004~0.080 mg/kg添加水平内，氰霜唑和CCIM回收率分别为80.71%~103.27%和76.62%~100.20%；相对标准偏差分别为4.14%~11.15%和3.24%~11.16%，检出限和定量限分别为0.001 5~0.003 8 mg/kg和0.003 0~0.007 9 mg/kg。该方法简单快速、分析时间短、灵敏度及准确度高，能够满足快速定性、定量检测水果样品中氰霜唑及CCIM的残留量。

Abstract:

A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was established for the simultaneous determination of cyazofamid and its major metabolite 4-chloro-5-(4-methylphenyl )-1H-imidazol-2-nitrile (CCIM) to evaluate their safety in fruits. The sample was extracted with acetonitrile containing 1.0% acetate acid and purified with octadecylsilane bonded phase (C₁₈) powder and Florisil powder. Then the UPLC separation of sample was performed on Capcell PAK C18 column (150 mm×2.0 mm, 5 μm) and determined with multiple reaction monitoring mode (MRM) through HPLC-MS/MS. The results showed good linear relationships between the peak areas and the mass concentrations for both cyazofamid and CCIM in the range of 0.001~0.040 μg/mL (R≥0.999 3). When the spiked levels were between 0.004~0.080 mg/kg, the recoveries of cyazofamid and CCIM were in the range of 80.71%~103.27% and 76.62%~100.20%, respectively, and the relative standard deviations were between 4.14%~11.15% and 3.24%~11.16%, respectively. The LODs and LOQs of cyazofamid and CCIM in fruits were between 0.001 5~0.003 8 mg/kg and 0.003 0~0.007 9 mg/kg, respectively. The method was simple, rapid, high sensitivity and accurate, which could satisfy the rapid qualitative and quantitative detection of cyazofamid and CCIM residues in fruit samples.