分散固相萃取-GC-MS/MS法检测蒜粉中13种有机磷残留  

Determination of 13 Organophosphorus Pesticide Residues in Garlic Powder Using Dispersive Solid-phase Extraction and GC-MS/MS

作　　者：倪永付[1] 王勇[1] 闫秋成 朱莉萍[1] 

机构地区：[1]济宁出入境检验检疫局,山东济宁272000

出　　处：《食品与发酵科技》2014年第3期75-78,共4页Food and Fermentation Science & Technology

摘　　要：建立了分散固相萃取-气相色谱-串联质谱法检测蒜粉中13种有机磷农药残留的方法。样品经0.1%乙酸-乙腈提取,C18净化粉净化后,氮气吹干,用1.0mL乙酸乙酯定容,上机检测。采用TR-5MS(30m×0.25mm×25μm)色谱柱分离,在选择反应监测模式下检测,外标法定量。结果表明:13种有机磷农药在浓度0.02-1.0mg/L范围内线性关系良好,相关系数r=0.9910-0.9978,方法检测限为0.001-0.01mg/kg,定量限为0.005-0.02mg/kg。在不同添加水平下,其平均回收率为70-120%,变异系数为3.4-14.3%。A method was established to determine the 13 organophosphorus pesticide residues in garlic powder by dispersive solid-phase extraction and gas chromatography-tandem mass spectrometry method. The sample was ex-tracted by 0.1% acetic acid-acetonitrile. After being cleaned by C18 powder, and then dried by the nitrogen flow, the sample was dissolved in 1.0mL ethyl acetate and performed on TR-5MS （30m×0.25mm×25μm） column. The analysis was carried out in the select reaction monitoring mode and external standard method was used for quantifi-cation. The calibration curve of the 13 organophosphorus pesticides was good linear from 0.02 to 1.0mg/L with the correlation coefficient r=0.9910-0.9978, the detection limits of this method were 0.001~0.01mg/kg and the quantita-tive limits were 0.005-0.02mg/kg. In different concentrations, the average recoveries of this method were 70-120%and the variability coefficient were 3.4-14.3%.

关 键 词：分散固相萃取 气相色谱-质谱 质谱法 蒜粉 有机磷 残留 

分 类 号：TS207.53[轻工技术与工程—食品科学]