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

作　　者：符灵梅 王玉健 徐莉 纪少凡 FU Lingmei;WANG Yujian;XU Li;JI Shaofan(Technology Center of Haikou Customs,Haikou 570311,China)

机构地区：[1]海口海关技术中心,海南海口570311

出　　处：《食品与生物技术学报》2022年第9期93-103,共11页Journal of Food Science and Biotechnology

基　　金：海南省重点研发计划项目(ZDYF2019106);海关技术规范计划项目(2019B111)

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(C_(18))粉末和弗罗里硅土粉末净化后,以Capcell PAK C_(18)色谱柱(150 mm×2.0 mm,5μm)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0.001~0.040μg/mL时,质量浓度与峰面积呈良好的线性关系(R≥0.9993),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0.0015~0.0038 mg/kg和0.0030~0.0079 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。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(C_(18))powder and Florisil powder.Then the UPLC separation of sample was performed on Capcell PAK C_(18) column(150 mm×2.0 mm,5μm)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 0.001~0.040μg/mL(R≥0.9993).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 0.0015~0.0038 mg/kg and 0.0030~0.0079 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.

关 键 词：超高效液相色谱-串联质谱法 氰霜唑 农药残留 

分 类 号：S481.8[农业科学—农药学]