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固相萃取-液相色谱串联质谱测定枸杞中有机磷农药残留 被引量:13

Solid Phase Extraction Followed by Liquid Chromatography Tandem Mass Spectrometry for the Determination of Organophosphorus Pesticide Residues in Lycium barbarum L.
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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.
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)
关键词 固相萃取 液相色谱-串联质谱 有机磷农残 枸杞 solid-phase extraction LC-MS/MS organophosphorus pesticide residues Lycium barbarum L
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