文献类型：期刊文献

中文题名：分散固相萃取-高效液相色谱-串联质谱法测定铁皮石斛中8种有机磷农药残留

英文题名：Determination of 8 organophosphorus pesticides in fresh Dendrobium officinale by dispersive solid-phase extraction method and high performance liquid chromatography-tandem mass spectrometry

作者：钟冬莲[1,2] 汤富彬[2] 莫润宏[2] 沈丹玉[2] 张延平[2] 李祖光[1]

第一作者：钟冬莲

机构：[1]浙江工业大学化学工程学院;[2]中国林业科学研究院亚热带林业研究所

年份：2017

卷号：36

期号：5

起止页码：571-575

中文期刊名：分析试验室

外文期刊名：Chinese Journal of Analysis Laboratory

收录：CSTPCD;;北大核心:【北大核心2014】；CSCD:【CSCD2017_2018】；

基金：浙江省省院合作林业科技项目(2014SY12)资助

语种：中文

中文关键词：铁皮石斛;高效液相色谱-串联质谱法;分散固相萃取;有机磷农药残留

外文关键词：Dendrobium officinale ; High performance liquid chromatography-tandem mass

分类号：I84

摘要：建立了分散固相萃取结合高效液相色谱-串联质谱法(d-SPE-HPLC-MS/MS)测定铁皮石斛栽培过程中可能使用的8种有机磷农药。前处理采用Qu ECh ERS方法,样品先经水浸润,用乙腈高速均质提取,经分散固相萃取净化,Waters Atlantis T3色谱柱分离,电喷雾串联质谱多反应监测模式测定,基质匹配标准曲线外标法定量。8种有机磷农药在测定的范围内线性关系良好(R>0.997),在10,50,100μg/kg添加水平下8种农药的回收率范围为75.9%~117.8%,相对标准偏差在2.1%~12.3%(n=6)之间;检出限和定量限分别为0.15~5.47μg/kg和0.84~8.52μg/kg。该方法样品前处理简单、快速、选择性好、灵敏度高,适合于铁皮石斛鲜样中多种有机磷农药的快速测定。
In this study, dispersive solid-phase extraction （d-SPE） combined with high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） method was developed for the determination of 8 organophosphorus pesticides in Dendrobium officinale samples. The samples were prepared by the QuEChERS （quick, easy, cheap, effective, rugged and safe）method, soaked by water and then homogeneously extracted with acetonitrile. The extracts were cleaned up by d-SPE using PSA, separated on a Waters Atlantis T3 column and analyzes by HPLC-MS/MS under multiple reaction monitoring mode. Matrix matching curve external standard method was used for quantification. The method shows excellent linearities （ R 〉 0. 997 ） for all compounds in a certain concentration range. The recoveries at three spiked levels of 10, 50 and 100 μg/kg ranged from 75.9% to 117.8% with the relative standard deviations （RSD） （ n = 6 ） from 2. 1% to 12.3 %. The limits of detection （LOD） and the limits of quantification （LOQ） of 8 pesticide residues were in the range of 0. 15 -5.47μg/kg and 0. 84 ~ 8.52 μg/kg, respectively. The method has been proven to be simple, quick, sensitive and suitable for determination of organophosphorus pesticides in fresh Dendrobium officinale samples.