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采用一步法快速、简便、廉价、有效、耐用、安全法结合超高效液相色谱四极杆轨道阱质谱法对牧草中的 206 种农药进行多残留分析。

Multi-residue analysis of 206 pesticides in grass forage by the one-step quick, easy, cheap, effective, rugged, and safe method combined with ultrahigh-performance liquid chromatography quadrupole orbitrap mass spectrometry.

机构信息

Key Laboratory of Food Quality and Safety for State Market Regulation, Chinese Academy of Inspection and Quarantine, Beijing, P. R. China.

Laboratory of Heilongjiang Feihe Dairy Co. Ltd, Heilongjiang Feihe Dairy Co., Ltd., Qiqihar, P. R. China.

出版信息

J Sep Sci. 2022 Jul;45(14):2520-2528. doi: 10.1002/jssc.202200066. Epub 2022 May 21.

Abstract

A novel method for detecting pesticide multi-residue in grass forage (alfalfa and oat) was established based on the one-step automatic extraction and purification technology of quick, easy, cheap, effective, rugged, and safe combined with ultrahigh-performance liquid chromatography quadrupole Orbitrap high-resolution mass spectrometry. The crushed sample was extracted with acetonitrile with 1% acetate, followed by a cleanup step with a primary-secondary amine, octadecylsilane, and graphitized carbon black. The extraction and purification were carried out using the one-step automatic pretreatment equipment. The target pesticides were acquired in positive ion electrospray ionization mode and full scan/data dependent secondary scan mode. The calibration curve shows good linearity over the corresponding concentration range, with the coefficient of determination greater than 0.99. The screening detection limits were 0.5-50 μg/kg, and the limit of quantification for the 206 pesticides was set at 1-50 μg/kg. At the spiking levels of one, two, and 10 times of limit of quantification, more than 95% of pesticides had recovery between 70-120%, with a relative standard deviation ≤20%. The method was proved to be simple, rapid, high-sensitivity, and could be routinely used for the high throughput screening and quantitative analysis of pesticide residues in alfalfa and oat.

摘要

基于一步自动提取和净化技术,结合快速、简便、廉价、有效、坚固和安全的特点,建立了一种检测草饲料(苜蓿和燕麦)中农药多残留的新方法,与超高效液相色谱四极杆轨道阱高分辨率质谱联用。将粉碎的样品用 1%醋酸乙腈提取,然后用伯仲胺、十八烷基硅烷和石墨化炭黑进行净化。采用一步式自动预处理设备进行提取和净化。目标农药采用正离子电喷雾电离模式和全扫描/数据依赖二次扫描模式进行采集。校准曲线在相应浓度范围内具有良好的线性关系,相关系数大于 0.99。筛选检测限为 0.5-50μg/kg,206 种农药的定量限设定为 1-50μg/kg。在定量限的 1、2 和 10 倍添加水平下,超过 95%的农药回收率在 70-120%之间,相对标准偏差≤20%。该方法简单、快速、灵敏度高,可用于苜蓿和燕麦中农药残留的高通量筛选和定量分析。

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