超高效液相色谱-串联质谱法测定浓缩苹果汁中61种农药残留量  

Determination of 61 pesticide residues in concentrated apple juice using ultra performance liquid chromatography-tandem mass spectrometry

作　　者：何强 刘学芝 孔祥虹 李建华 

机构地区：[1]陕西出入境检验检疫局,西安710068

出　　处：《分析试验室》2015年第3期300-306,共7页Chinese Journal of Analysis Laboratory

基　　金：国家质检总局科研项目(2014IK128)资助

摘　　要：建立了浓缩苹果汁中61种农药残留量的超高效液相色谱-串联质谱检测方法。样品经Na2HPO4缓冲液稀释、Na OH溶液调节p H后用乙腈提取,N-丙基乙二胺（PSA）固相萃取柱净化,采用ACQUITY UPLC HSS T3色谱柱分离,甲醇-0.1%甲酸溶液梯度洗脱,多反应监测（MRM）模式测定,外标法定量。61种农药在0.01~0.5 mg/L浓度范围内线性关系良好,相关系数均大于0.98,检出限在0.23×10-3~2.9×10-3mg/kg范围内。在浓缩苹果汁中分别添加0.01,0.02,0.05 mg/kg 3个浓度水平,进行加标回收率实验,平均回收率均在77.5%~103.5%范围内,相对标准偏差均低于15%,方法的灵敏度、准确性、重现性均符合农药残留检测的要求。An ultra performance liquid chromatography tandem mass spectrometric method（ UPLC-MS / MS） has been developed for the determination of 61 pesticide residues in concentrated apple juice（ AJC）. The sample was deluted with disodium hydrogen phosphate buffer solution,and adjusted p H to 8 ~ 9,and then extracted by acetonitrile. The extraction solution was cleaned by a N-propyl ethylenediamine（ PSA） solid-phase extraction column. UPLC was performed on a ACQUITY UPLC HSS T3 column using a gradient methanol-aqueous solution containing 0. 1% formic acid system as mobile phase,and MS / MS was performed with multiple reaction monitoring（ MRM） mode. Quantitation was carried out using an external standard method. The calibration curves of the 61 pesticides were linear in the range of 0. 01 ~ 0. 5 mg / L with linear correlation coefficients not less than 0. 98,and the detection limits were between 0. 23 × 10-3mg / kg to 2. 9 × 10-3mg / kg. The average recoveries of all the pesticides were in the range of 77. 5% to 103. 5% at three spiked levels of 0. 01,0. 02 and0. 05 mg / kg in concentrated apple juice,and the relative standard deviations were lower than 15%. The sensitivity,accuracy and repeatability of the method all meet the requirements of pesticide residual analysis.

关 键 词：浓缩苹果汁 农药残留 超高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学]