固相萃取-液相色谱串联质谱测定枸杞中有机磷农药残留

采用固相萃取-液相色谱串联质谱仪,建立枸杞中9种有机磷农药的快速测定方法。样品经乙腈提取,过Carbon/NH2固相萃取柱净化,氮吹至干,残留物用乙腈-水（3：2,V/V）溶解后测定,采用正离子扫描方式进行仪器方法学研究,确定监测离子对,进行SRM模式定性定量分析。该方法的检出限（LOD）为0.12～9.8μg/L;在10～200μg/L范围内线性关系良好（r〉0.9961）。在20～100μg/L的添加水平上,9种有机磷农药的平均回收率在80.7%～122.4%之间,相对标准偏差（RSD）为2.75%～14.7%。该方法操作简单,灵敏度高,可用于枸杞中9种有机磷农残的测定。

Solid Phase Extraction Followed by Liquid Chromatography Tandem Mass Spectrometry for the Determination of Organophosphorus Pesticide Residues in Lycium barbarum L.

This study developed a quick and specific method for the identification and quantification of pesticide residues in Lycium barbarum L.Samples were extracted using acetonitrile,and extracts were cleand up by solid-phase extraction on a Carbon/NH2(SPE) cartridge,blowed to dryness by nitrogen,and dissolved in a mixture of acetonitrile and water(3:2,V/V) prior to LC-MS/MS analysis in a select reaction monitoring(SRM) mode.The limits of detection(LODs) ranged in 0.12～9.8μg/L.The regression equations were well linear between 10.0 and 200.0 μg/L for these steroids(r>0.9961).The recoveries ranged from 80.7% to 122.4% with a RSD of 2.75%～14.7% at three spiked levels of 20～100μg/L.The method is simple,sensitive and rapid and therefore can be used for the determination of organophosphorus pesticide residues in Lycium barbarum L.