摘要
将固相支撑液液萃取与超高效液相色谱串联质谱法结合,建立生乳中32种农药残留的快速检测方法,为保障生乳食品安全提供技术支持。样品加入乙腈沉淀蛋白,高速离心分离,上清液用固相支撑液液萃取小柱净化,C18色谱柱梯度洗脱分离后,经串联质谱电喷雾模式扫描,多反应监测模式检测,以基质匹配校准曲线外标法定量。结果表明,32种目标物在一定范围内线性关系良好,相关系数大于0.9962,检出限为0.1~2.5μg/kg,定量限为0.3~7.5μg/kg,平均回收率为69.4%~113.8%,相对标准偏差(n=6)小于8.2%。该方法简单、快速、可靠,适用于生乳中32种农药残留的测定。
To provide scientific support for guaranteeing food safety in raw milk,a rapid method for the determination of pesticide residues in raw milk was developed using supported liquid extraction technique and ultra-performance liquid chromatography tandem mass spectrometry.The sample was precipitated with acetonitrile and then separated by high speed centrifugation.The supernatant was purified by SLE column.Separation of pesticide residues was achieved by a CORTECS C18 column.Pesticide residues were detected by ultra-performance liquid chromatography tandem mass spectrometry with electrospray ionization in the multiple reaction monitoring mode,and the quantification was accomplished by external standard method of matrix standard curve.Method validation revealed satisfactory linearities with correlation coefficients higher than 0.9962,and limits of detection and quantification for target compounds were 0.1~2.5μg/kg and 0.3~7.5μg/kg,the average recoveries at three spiked levels were in the range of 69.4%~113.6%with relative standard deviation(RSD,n=6)less than 8.2%.This method is simple,quickly and reliable,and shows great promise for detecting 32 different pesticide residues in raw milk.
作者
邓龙
周思
黄佳佳
曾上敏
张静文
DENG Long;ZHOU Si;HUANG Jiajia;ZENG Shangmin;ZHANG Jingwen(Guangdong Food and Drug Vocational College,Guangzhou 510520,China;Guangzhou Centre for Disease Control and Prevention,Guangzhou 510440,China)
出处
《食品工业科技》
CAS
北大核心
2023年第17期360-366,共7页
Science and Technology of Food Industry
基金
广东省医学科学技术研究基金项目(A2020197,A2022496)
广东省普通高校青年创新人才项目(2020KQNCX172)
广东食品药品职业学院自然科学研究项目(2019ZR21,2020ZR16,2022ZR12)。
