固相萃取-液相色谱串联质谱测定枸杞中有机磷农药残留  

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

作　　者：梁月香[1] 王晓菁[1] 姜瑞[1] 吴燕[1] 牛艳[1] 

机构地区：[1]农业部枸杞产品质量监督检验测试中心,宁夏银川750002

出　　处：《山东林业科技》2011年第6期1-4,共4页Journal of Shandong Forestry Science and Technology

基　　金：国家科技支撑项目(2009BAI72B00);宁夏回族自治区自然科学基金项目(NZ1046)

摘　　要：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。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（r0.9961）.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.

关 键 词：固相萃取 液相色谱-串联质谱 有机磷农残 枸杞 

分 类 号：Q503[生物学—生物化学]