超高效液相色谱-串联质谱法测定花椰菜中氯虫苯甲酰胺和多杀霉素的残留

Determination of Chlorantraniliprole and Spinosad Residues in Cauliflower Using Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry

本研究建立了一种运用超高效液相色谱-串联质谱(UPLC-MS/MS)快速检测花椰菜中氯虫苯甲酰胺和多杀霉素残留的方法。样品经乙腈提取后用N-丙基乙二胺(PSA)和石墨化碳黑(GCB)净化,流动相为乙腈和水溶液,梯度洗脱。采用电喷雾正离子(ESI^(+))电离,多反应监测模式(MRM)进行定量分析,基质匹配标准曲线外标法定量。结果表明,氯虫苯甲酰胺、多杀霉素A和多杀霉素D的定量限(LOQ)分别为0.050、0.039、0.011 mg/kg。在0.05~0.5 mg/mL范围内,氯虫苯甲酰胺、多杀霉素A和多杀霉素D的质量浓度与峰面积间线性关系良好(R^(2)>0.99)。3种药剂在花椰菜中的回收率为96%~107%之间,相对标准偏差(RSD)在1.4%~8.4%之间。该方法简单、快速,灵敏度及正确度高,可满足花椰菜中氯虫苯甲酰胺和多杀霉素残留的检测要求。

A rapid method for analyzing chlorantraniliprole and spinosad residues in cauliflower was developed by using ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Cauliflower was extracted with acetonitrile and cleaned up with N-propyl ethylenediamine(PSA)and graphitized carbon black(GCB).Acetonitrile and water were used as mobile phase.Electrospray ionization in positive ion mode was selected,the detection mode was multi-reaction monitoring,and the external standard method was used for quantification.The method showed that the limit of quantification(LOQ)of chlorantraniliprole,spinosad A and spinosad D was 0.050,0.039 mg/kg and 0.011 mg/kg.There was a good linear relationship between the mass concentration and peak area of the three tested compounds(R^(2)>0.99)in the range of 0.05-0.5 mg/mL.The average recoveries were 96%-107%in the cauliflower samples,with relative standard deviations(RSD)of 1.4%-8.4%.The method is simple,rapid,sensitive,and accurate,which meets the requirement of the determination of chlorantraniliprole and spinosad residues in cauliflower.