分散固相萃取-超高效液相色谱-串联质谱法测定果蔬、牛奶、植物油和动物肌肉中残留的61种有机磷农药

建立了果蔬、牛奶、植物油和动物肌肉中61种有机磷农药多残留的分析方法。果蔬和牛奶样品用乙腈均质提取,盐析分配;植物油样品用正己烷溶解,乙腈萃取;动物肌肉样品用正己烷配合乙腈-水溶液均质提取,盐析分配。各提取法得到的提取液采用C18和Primary Secondary Amine (PSA)粉末分散固相萃取净化,超高效液相色谱-串联质谱仪(UPLC-MS/MS)分析,采用电喷雾离子化正离子方式(ESI+)及多反应监测模式(MRM)测定,基质匹配标准溶液外标法定量。方法的定量限(S/N≥10)均达到0.01 mg/kg;回收率为62.8%～107%,相对标准偏差为4.2%～19%。该方法准确、灵敏、快速,可满足多种食品中有机磷农药残留的检测要求。

Determination of 61 organophosphorous pesticide residues in fruits, vegetables, milk, vegetable oils and animal muscles by dispersive solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry

A dispersive solid-phase extraction coupled with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) method was developed for the determination of 61 organophosphorous pesticide residues in fruits,vegetables,milk,vegetable oils and animal muscles.The fruit,vegetable and milk samples were extracted with acetonitrile and separated with salting out method;vegetable oil samples were dissolved by n-hexane,and extracted with acetonitrile;animal muscle samples were extracted with acetonitr...