摘要
针对干果果肉基质含水量低、含糖量较高等特点,建立了改进的分散固相萃取结合超高效液相色谱-质谱/质谱法（UPLC-MS/MS）测定干果果肉培育过程中可能使用的56种农药残留量。样品经水浸润,以0.1%甲酸-乙腈提取,改进的分散固相萃取法（PSA）净化,液相色谱-质谱/质谱法检测,基质匹配标准曲线外标法定量。56种农药在10～500μg/L范围内线性关系良好,相关系数均大于0.990,在5,10和50μg/kg添加水平下56种农药回收率范围为60.4%～127.9%;相对标准偏差在1.1%～20%（n=6）之间;检出限和定量限分别为0.1～1.0μg/kg和0.3～3.1μg/kg。方法适合于干果果肉中56种农残检测。
A modified dispersive solid-phase extraction（ d-SPE） method followed by ultra-high liquid chromatography-tandem mass spectrometry（ UPLC-MS / MS） analysis was developed for the determination of 56 pesticide residues in dried fruit pulps. Samples were soaked by water and then 0. 1% formic acid-acetonitrile was added to extract the analytes. The extracts were cleaned up by d-SPE using primary secondary amine（ PSA）. The modified d-SPE method could not only enhance penetration of acetonitrile but also remove most of saccharides,so the efficiency of extraction was improved significantly. The analytes were separated by liquid chromatography and determined by mass spectrometry. Matrix matching curve external standard method was used for quantification.The linearity of all the analytes was good in the concentration ranges of 10 μg / L to 500 μg / L with correlation efficient larger than 0. 990. The recoveries at three spiked levels of 5,10 and 50 μg / kg ranged from 60. 4% to127. 9% with the relative standard deviations（ RSD）（ n = 6） from 1. 1% to 20%. The limit of detection（ LOD）and the limit of quantification（ LOQ） of 56 pesticide residues were in the range of 0. 1 ～ 1. 0 μg / kg and 0. 3 ～3. 1 μg / kg,respectively. The method has been proven to be sensitive,simple,quick,economical and suitable for determination of 56 pesticide residues in dried fruit pulps.
出处
《分析试验室》
CAS
CSCD
北大核心
2016年第3期287-292,共6页
Chinese Journal of Analysis Laboratory
基金
国家质检总局科技计划项目(2014IK115)资助
关键词
干果果肉
超高效液相色谱法-质谱/质谱法
分散固相萃取法
农药残留
Dried fruit pulps
Ultra-high liquid chromatography-tandem mass spectrometry（UPLC-MS / MS）
Dispersive solid-phase extraction（d-SPE）
Pesticide residues
