QuEChERS-高效液相色谱-串联质谱法测定毛豆中常用21种农药残留  

Determination of 21 kinds of pesticide residues in soybean by Qu ECh ERS-high performance liquid chromatography-tandem mass spectrometry

作　　者：钟莉萍[1] 徐敦明[1] 赖国银[1] 张志刚[1] ZHONG Li-Ping XU Dun-Ming LAI Guo-Yin ZHAGN Zhi-Gang(Technical Center of Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China)

机构地区：[1]厦门出入境检验检疫局检验检疫技术中心,厦门361026

出　　处：《食品安全质量检测学报》2016年第11期4633-4640,共8页Journal of Food Safety and Quality

基　　金：福建省自然基金项目(2016J05045);行业标准项目(2016B111)~~

摘　　要：目的：建立液相色谱-串联质谱法同时检测毛豆中21种常用农药残留的分析方法。方法样品以乙腈-甲酸（99：1, V：V）作为提取剂,经QuEChERS方法前处理,采用Phenomenex的Kinetex C18色谱柱（50 mm×2.1 mm,2.6μm,100？）分离,以乙腈-0.1%甲酸水溶液为流动相梯度洗脱,以电喷雾电离（ESI）、正离子模式和负离子模式2种多反应监测（MRM）模式检测,外标法定量。结果21种农药在5~200 ng/mL范围内,线性相关系数均大于0.99,线性良好。分析目标物添加水平为0.01~0.10 mg/kg 时,回收率范围为73%~113%, RSD 范围为1.3%~10.9%,符合残留分析的要求。21种农药的定量下限为0.01 mg/kg。结论该方法的提取简便,基质分散效果好,灵敏度满足国内外限量标准的要求,适合毛豆中常用农药残留的同时测定。Objective To establish a method for the simultaneous detection of 21 kinds of pesticide residues in soybean by liquid chromatography-tandem mass spectrometry. Methods With acetonitrile/formic acid （99：1, V：V） as extraction agent, samples were performed by QuEChERS method, separated by Kinetex C18 phenomenex chromatographic column （50 mm×2.1 mm, 2.6μm, 100 ？） and gradient eluted with acetonitrile and 0.1%formic acid as the mobile phase. After electrospray ionization, samples were detected under positive and negative multiple reaction monitoring （MRM） modes, and quantified by external standard method. Results The 21 kinds of pesticides had good linearities in the range of 5~200 ng/mL and the linear correlation coefficients were greater than 0.99. When the target addition level was 0.01~0.10 mg/kg, the recovery rates were in the range of 73%~113%and the RSDs were 1.3%~10.9%, according with the requirements of residue analysis. The limits of determination and the limits of quantification of the 21 kinds of pesticides were 0.01 mg/kg. Conclusion The established method has the advantages of simple extraction and good matrix dispersion effect, and can meet the requirements for the simultaneous determination of pesticide residues in soybean.

关 键 词：高效液相色谱-串联质谱法 毛豆 农药残留 

分 类 号：TS214[轻工技术与工程—粮食、油脂及植物蛋白工程] O657.63[轻工技术与工程—食品科学与工程]