固相萃取结合气相色谱-三重四极杆质谱法测定高酸水果中48种农药残留  

Determination of 48 Pesticide Residues in High-acidity Fruits by Gas Chromatography-Triple Quadrupole Mass Spectrometry Combined with Solid-phase Extraction

作　　者：张博伦 庞国芳[1,2] 冯春 李建勋[1,2] 吴兴强 胡雪艳 范春林[2] ZHANGBo- lun;PANGGuo- fang;FENG Chun;LI Jian- xun;WUXing- qiang;HU Xue- yan;FAN Chun- lin(College of Food and Chemical Engineering,Beijing Technology and Business University,Beijing 100048,China;Chinese Academy of Inspection and Quarantine,Beijing 100176,China;College of Chemistry and Environmental Science,Hebei University,Baoding 071002,China)

机构地区：[1]北京工商大学食品学院,北京100048 [2]中国检验检疫科学研究院,北京100176 [3]河北大学化学与环境科学学院,河北保定071002

出　　处：《分析测试学报》2018年第6期653-659,共7页Journal of Instrumental Analysis

基　　金：国家科技基础性工作专项(2015FY111200)

摘　　要：将固相萃取与气相色谱-三重四极杆质谱(GC-MS/MS)联用,建立了准确测定高酸水果基质中48种农药残留的方法。样品经酸化乙腈提取,Carbon NH2和氨基填料柱净化,旋转蒸发浓缩萃取后,采用GCMS/MS分析。以柚子、橙子、菠萝、山楂为基质,考察了提取剂种类、提取时间、萃取柱填料种类对萃取结果的影响。结果表明,48种农药在1.0~100.0μg/kg范围内线性关系良好,定量下限为1.0~10.0μg/kg。农药在4种水果中3个加标水平下的平均回收率为70.7%~118.0%,相对标准偏差(n=5)不大于9.7%。该方法检测范围广、定量准确、检出限低。应用所建立的方法对市售水果样品进行检测,结果较好。A gas chromatography-triple quadrupole mass spectrometric（ GC-MS/MS） method for the determination of 48 pesticide residues in high-acidity fruits was developed using solid-phase extraction as sample preparation method. The samples were extracted with acetonitrile containing 1%acetic acid,purified with a Carbon NH2 and Pro Elut NH2 solid-phase extraction column,and analyzed by GC-MS/MS. Effects of different kinds of extractants,extraction times and types of SPE column on the extraction efficiency were investigated by using pomelo,orange,pineapple and hawthorn matrixes. The results showed that the calibration curves of 48 pesticides were linear in the range of1. 0-100. 0 μg/kg with limits of quantitation of 1. 0-10. 0 μg/kg. The average recoveries for 48 pesticides in four kinds of fruits（ pomelo,orange,pineapple and hawthorn） ranged from 70. 7% to118. 0% with relative standard deviations（ RSD,n = 5） not more than 9. 7%. With wide detection range,high precision and low detection limit,the method was successfully applied in the detection of commercially available fruit samples.

关 键 词：固相萃取(SPE) 气相色谱-三重四极杆质谱 农药残留 水果 

分 类 号：O657.3[理学—分析化学] F767.2[理学—化学]