QuEChERS-超高效液相色谱串联质谱法测定水稻中氯虫苯甲酰胺和吡蚜酮残留量

Determination of residues of chlorantraniliprole and pymetrozine in rice by QuEChERS-UPLC-MS/MS

[目的]建立并优化基于超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测水稻中氯虫苯甲酰胺和吡蚜酮的分析方法。[方法]糙米样品采用乙腈-乙酸溶液提取,稻壳和秸秆样品采用乙腈-氨水提取,C_(18)和N-丙基乙二胺(PSA)净化,流动相为甲醇和0.01%甲酸-0.05%氨水水溶液,采用ACQUITY UPLC■BEH C_(18)色谱柱进行分离。电喷雾正离子模式和多反应监测(MRM)模式采集,外标法定量。[结果]糙米、稻壳和秸秆中氯虫苯甲酰胺的平均回收率为91%~102%,相对标准偏差为1.0%~9.5%;吡蚜酮的平均回收率为73%~94%,相对标准偏差为1.1%~5.8%。氯虫苯甲酰胺和吡蚜酮在糙米中的定量限均为0.01 mg/kg,在稻壳和秸秆中的定量限均为0.02 mg/kg。氯虫苯甲酰胺和吡蚜酮在0.001~0.5 mg/L的范围内均具有良好的线性关系,相关系数分别为0.9996和0.9988。[结论]方法不仅操作简便、快速,而且具备高灵敏度、高准确度和高精密度的特点,完全符合农作物中农药残留分析要求。建立的分析方法可广泛应用于水稻中氯虫苯甲酰胺和吡蚜酮的残留分析,为农产品质量安全提供有力保障。

[Aims]This study aims to establish and optimize an analytical method based on ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)for simultaneous detection of chlorantraniliprole and pymetrozine in rice.[Methods]Brown rice samples were extracted with acetonitrile-acetic acid solution,while rice husk and straw samples were extracted with acetonitrile-aqueous ammonia solution.The extracts were purified by C_(18)and N-propyl ethylenediamine(PSA).ACQUITY UPLC■BEH C_(18)chromatographic column was used for separation and the mobile phase was methanol and 0.01%formic acid-0.05%ammonia aqueous solution.Electrospray ionization in positive ion mode was selected,the detection mode was multiple reaction monitoring(MRM),and external standard method was used for quantification.[Results]The average recoveries of chlorantraniliprole in brown rice,rice husk and straw were 91%-102%,with relative standard deviations of 1.0%-9.5%.For pymetrozine,the average recoveries were 73%-94%,with relative standard deviations of 1.1%-5.8%.The limits of quantitation for chlorantraniliprole and pymetrozine were both 0.01 mg/kg in brown rice,and 0.02 mg/kg in rice husk and straw.Both chlorantraniliprole and pymetrozine exhibited good linear relationships within the range of 0.001-0.5 mg/L,with correlation coefficients of 0.9996 and 0.9988,respectively.[Conclusions]This method is not only simple and rapid to operate but also exhibits high sensitivity,accuracy and precision,fully meeting the requirements for pesticide residue analysis in crops.Therefore,the analytical method established in this study can be widely applied to the residue analysis of chlorantraniliprole and pymetrozine in rice,providing a strong support for the quality and safety of agricultural products.