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高效液相色谱-串联质谱法快速一步法净化分析辣椒、辣椒粉及其酱制品中 47 种农药残留。

Rapid single-step cleanup method for analyzing 47 pesticide residues in pepper, chili peppers and its sauce product by high performance liquid and gas chromatography-tandem mass spectrometry.

机构信息

Department of Applied Chemistry, College of Science, China Agricultural University, Beijing 100193, China.

Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China.

出版信息

Food Chem. 2019 May 1;279:237-245. doi: 10.1016/j.foodchem.2018.12.017. Epub 2018 Dec 11.

Abstract

A novel rapid single-step cleanup method combined with quick, easy, effective, rugged, and safe (QuEChERS) extraction approach for determining multi-pesticide residues was developed. For the single-step QuEChERS (sin-QuEChERS) cleanup procedure, a specified cartridge was fitted within an extraction centrifuge tube for removing non-target substances. Multi-walled carbon nanotubes (MWCNTs) and Primary Secondary Amine (PSA) mixed with salts functioned as absorbents. Method validation was applied on 47 representative pesticides in pepper, chili peppers and chili sauce by LC-MS/MS and GC-MS/MS detection. Compared to the original QuEChERS method, the Sin-QuEChERS method was fast and convenient without any further vortex or centrifugation. Satisfactory recoveries of most pesticides at two concentration levels were in the range of 70-120% (except for pyrimethanil) with relative standard deviations (RSDs n = 5) lower than 17%. The limit of quantification (LOQs) for the 47 pesticides were 0.01 mg/kg in three matrices. Sin-QuEChERS method was successfully applied to monitor the market multi-residues.

摘要

开发了一种新型的快速单步净化方法,结合快速、简便、有效、耐用和安全(QuEChERS)提取方法,用于测定多种农药残留。对于单步 QuEChERS(sin-QuEChERS)净化程序,在提取离心管内安装了指定的筒式过滤器,用于去除非目标物质。多壁碳纳米管(MWCNTs)和与盐混合的初级仲胺(PSA)用作吸附剂。通过 LC-MS/MS 和 GC-MS/MS 检测,对胡椒、辣椒和辣椒酱中的 47 种代表性农药进行了方法验证。与原始的 QuEChERS 方法相比,Sin-QuEChERS 方法快速便捷,无需进一步涡旋或离心。在两个浓度水平下,大多数农药的回收率均在 70-120%范围内(除嘧啶苯胺外),相对标准偏差(RSD,n=5)低于 17%。在三种基质中,47 种农药的定量限(LOQs)均为 0.01 mg/kg。Sin-QuEChERS 方法成功应用于监测市场上的多残留。

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