新疆农食产品基质中亚砜磷和溴氰虫酰胺测定的方法学研究

Research on the Methodology for Detection of Oxydemeton-methyl and Cyantraniliprole in the Matrix of Xinjiang Agricultural and Food Products

建立了QuEChERS前处理方法、液相色谱-串联质谱法(HPLC-MS/MS)同时检测新疆农食产品中亚砜磷和溴氰虫酰胺残留量的分离与定性定量检测确证方法。样品经乙腈提取,采用硅胶键合季铵基团(SAX)和聚苯乙烯-二乙烯苯(PEP)吸附剂净化。以0.1%(v/v)甲酸水-乙腈梯度洗脱,采用液相C18色谱柱分离,电喷雾正离子电离(ESI+),多重反应监测模式(MRM)检测。结果表明:亚砜磷的线性范围为1~50 ng/mL,溴氰虫酰胺的线性范围为4~200 ng/mL,线性关系良好(r> 0.996),二者的定量限分别为1.0μg/kg、4.0μg/kg。10种新疆农食产品基质在1倍、2倍、5倍和10倍的LOQ添加水平下(n=6),亚砜磷的回收率为64.6%~96.2%,相对标准偏差在1.0%~15.2%之间;溴氰虫酰胺的回收率在67.6%~120.2%,相对标准偏差0.8%~17.9%,该方法高效、快捷、灵敏度高,准确度和精密度均符合农药残留检测方法学要求,这为新疆农食产品中亚砜磷和溴氰虫酰胺的科学监控和制定标准提供了数据参考和技术支持。

A method for the simultaneous determination of oxydemeton-methyl and cyantraniliprole residues in Xinjiang agricultural and food products was developed using QuEChERS pretreatment followed by liquid chromatography-tandem mass spectrometry(HPLC-MS/MS). The samples were extracted with acetonitrile and purified using silica gel bonded with quaternary ammonium groups(SAX) and polystyrene-divinylbenzene(PEP) adsorbents. Separation was achieved using a liquid-phase C18 chromatographic column with a gradient elution of 0.1%(v/v) formic acid in water and acetonitrile, and detected in positive electrospray ionization(ESI+)mode with multiple reaction monitoring(MRM). Results indicated a good linear relationship within the range of 1-50 ng/mL for oxydemeton-methyl and 4-200 ng/mL for cyantraniliprole(r 0.996). The quantification limits for both were 1.0 μg/kg and 4.0 μg/kg respectively. In ten kinds of Xinjiang agricultural and food product matrices, at 1×, 2×, 5×, and 10× LOQ levels(n = 6), the recovery rate of oxydemeton-methyl ranged from 64.6% to 96.2%, with a relative standard deviation of 1.0%-15.2%. The recovery rate of cyantraniliprole ranged from 67.6% to 120.2% with a relative standard deviation of 0.8%-17.9%. This method is efficient, quick,and highly sensitive. Its accuracy and precision meet the requirements for pesticide residue detection methodologies. This provides data references and technical support for scientific monitoring and standard-setting for oxydemeton-methyl and cyantraniliprole in Xinjiang agricultural and food products.