摘要
建立QuEChERS-气相色谱-串联质谱技术同时测定豇豆中6种菊酯农药(甲氰菊酯、氯氟氰菊酯、氟氯氰菊酯、氯氰菊酯、氟胺氰菊酯、氰戊菊酯)含量的快速检测方法。豇豆样品经乙腈提取,采样QuEChERS法进行净化,目标化合物经TG-5SILMS(30 m×0.25 mm,0.25μm)色谱柱分离,采用三重串联四级杆选择反应监测模式(selected reaction monitoring,SRM)进行定性定量分析,外标法定量。结果表明,6种农药在0.001~0.5 mg/L范围内线性关系良好,相关系数均大于0.99;在3个添加浓度水平(0.01,0.05,0.10 mg/kg)下,平均回收率在89.6%~106.9%之间;5次重复的相对标准偏差在4.0%~11.9%;甲氰菊酯、氟氯氰菊酯和氰戊菊酯的定量限为0.003 mg/kg,氯氟氰菊酯、氯氰菊酯和氟胺氰菊酯的定量限为0.0015 mg/kg。该方法操作简便,结果准确,能满足豇豆中6种菊酯农药残留检测的要求。
For the determination of 6 pyrethroid pesticide residues in cowpea(fenpropathrin,cyhalothrin,cyfluthrin,cypermethrin,fluvalinate,and fenvalerate),a rapid analysis method was established by QuEChERSgas chromatography-tandem mass spectrometry(QuEChERS-GC-MS/MS).The cowpea were extracted with acetonitrile,and purified by QuEChERS method.After that,the purification solution was separated by capillary GC columns TG-5SILMS(30 m×0.25 mm,0.25μm).A tandem quadrupole spectrometer operating in either full scan mode or in MS/MS mode for selected reaction monitoring(SRM)was used for the qualitative and quantitative analysis of the constituents,respectively.The results showed that the average recoveries of two pesticides were 89.6%~106.9%when the spiked levels were 0.01,0.05,and 0.10 mg/kg,with relative standard deviations(RSDs)in the range of 4.0%~11.9%(n=5).The calibration curve showed a good linearity in the ranges of 0.001~0.5 mg/L,with the coefficient of determination was over 0.99.The limits of quantitation(LOQ)for fenpropathrin,cyfluthrin,and fenvalerate were 0.003 mg/kg;and for cyhalothrin,cypermethrin,and fluvalinate were 0.0015 mg/kg,respectively.This method is simple to operate,and accurate for the results,and also can meet the requirements for determination of 6 pyrethroid pesticide residues in cowpea.
作者
张群
马晨
秦安丽
段云
郇志博
吴琼
ZHANG Qun;MA Chen;QIN Anli;DUAN Yun;HUAN Zhibo;WU Qiong(Analysis and Testing Center,CATAS,Haikou 571101,China;Laboratory of Quality and Safety Risk Assessment for Tropical Products,Ministry of Agriculture and Rural Affairs,Haikou 571101,China;Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables,Haikou 571101,China)
出处
《中国测试》
CAS
北大核心
2021年第2期63-67,共5页
China Measurement & Test
基金
海南省自然科学基金(318MS089)
国家农产品质量安全风险评估专项课题(GJFP201900605)
海南省自然科学基金高层次人才资助项目(320RC679)
海南省院士创新平台科研专项(YSPTZX202021)。
