四极杆/静电场轨道阱高分辨质谱在青椒中农药多残留快速筛查的应用  

Rapid Screening of Multi-residue Pesticides in Green Pepper by High-resolution Benchtop Q Exactive Mass Spectrometry

作　　者：陈达炜[1] 吕冰[1] 邹建宏[2] 杨欣[1] 苗虹[1] 赵云峰[1] 

机构地区：[1]国家食品安全风险评估中心/卫生部食品安全风险评估重点实验室,北京100021 [2]第二炮兵总医院,北京100088

出　　处：《分析测试学报》2014年第12期1327-1333,共7页Journal of Instrumental Analysis

基　　金：科技部国际合作项目(2011DFA31770)

摘　　要：建立了分散固相萃取法（d-SPE）萃取,高效液相色谱-四极杆/静电场轨道阱高分辨质谱快速筛查青椒中农药多残留的分析方法.样品采用乙腈提取,经N-丙基乙二胺（PSA）和C18分散固相萃取净化,以BEH C18色谱柱为分析柱,0.1％甲酸乙腈及含0.1％甲酸和4mmol/L甲酸铵水溶液作为流动相进行梯度洗脱分离.采用正、负离子切换,同时对欧盟青椒定性和定量考核样品进行快速筛查,并对定量考核样品筛查到的16种农药进行定量测定.16种农药在一定浓度范围内呈良好的线性关系,相关系数（r2）大于0.995,该方法的定量下限为0.4～2.0 μg/kg.在不同加标水平下的平均回收率为81.6％ ～ 116.5％,相对标准偏差为0.4％～7.5％.以欧盟青椒定量考核样品为研究对象,对其分别进行四极杆/静电场轨道阱高分辨质谱和三重四极杆质谱测定,结果表明,四极杆/静电场轨道阱高分辨质谱定量结果可与三重四极杆质谱结果相媲美.本方法简单、灵敏、准确,适用于农产品中农药多残留的快速筛查和分析测定,具有很好的实际应用价值.A dispersive solid phase extraction （d-SPE）/high-resolution benchtop Q Exactive mass spectrometric （HRMS） method was established for the rapid screening of pesticide multi-residue in green pepper.The samples were extracted with acetonitrile,and cleaned up by dispersive solid phase extraction with N-propyl ethlene diamine （PSA） and C18.The chromatographic analysis was performed on a BEH C18 column using acetonitrile（containing 0.1％ formic acid） and 4 mmol/L ammonium formate （containing 0.1％ formic acid） solution as mobile phases by a gradient elution program.The multi-residue pesticides were analyzed by Q Exactive high-resolution mass spectrometry in switching positive and negative modes,which were applied in rapid screening of pesticides for EU checking pepper samples.16 pesticide analytes were screened qualitatively from the checking pepper sample and were carried on the quantitative analysis.The method showed a good linearity in a certain concentration range for 16 pesticides with average recoveries of 81.6％-116.5％ and RSDs of 0.4％-7.5％.The limits of quantitation（LOQs） for 16 pesticides in pepper were between 0.4 μg/kg and 2.0 μg/kg.The method was simple,sensitive and accurate,and was suitable for the rapid screening of multi-residue pesticides in agricultural products.

关 键 词：高分辨质谱 农药 青椒 分散固相萃取 高效液相色谱 多残留 

分 类 号：O657.63[理学—分析化学] F767.2[理学—化学]