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采用分散固相萃取-液相色谱串联质谱法同时测定菰中 25 种农药残留

Simultaneous determination of 25 pesticides in Zizania latifolia by dispersive solid-phase extraction and liquid chromatography-tandem mass spectrometry.

机构信息

The Ningbo Academy of Agricultural Sciences, Ningbo, 315040, PR China.

SGS-CSTC Standards Technical Services (Ningbo) Co., Ltd., Ningbo, 315040, PR, China.

出版信息

Sci Rep. 2019 Jul 11;9(1):10031. doi: 10.1038/s41598-019-46523-y.

Abstract

An improved quick, easy, cheap, effective, rugged, and safe (QuEChERS) method combined with ultrapressure liquid chromatography tandem mass spectrometric method (UPLC-MS/MS) was developed to simultaneously determine 25 pesticides in Zizania latifolia. The samples were extracted with methanol(MeOH) and 0.1% formic acid (80:20, v/v) and cleaned with C absorbent and primary-secondary amine (PSA). LC separation was performed on a BEH C UPLC column under the condition of gradient elution with the mobile phase consisted of 0.5% formic acid (10 mM ammonium acetate)/MeOH. External standard calibration method with matrix-matched was used for quantification, and good linearity was obtained over a concentration range of 0.5-100 μg/l, with correlation coefficients greater than 0.9901. The limit of detection (LOD) and the limit of quantitation (LOQ) of the 25 pesticides were in the range of 0.2-1.0 µg/kg and 0.5-3.3 µg/kg, respectively. The recoveries ranged from 72% to 118%, and the relative standard deviations (RSDs) were less than 20%. Thus, the proposed method is suitable for the simultaneous determination of 25 pesticides in Z. latifolia.

摘要

建立了一种改进的 QuEChERS 方法,结合超高效液相色谱-串联质谱法(UPLC-MS/MS),用于同时测定菰中 25 种农药。样品用甲醇(MeOH)和 0.1%甲酸(80:20,v/v)提取,用 C 吸剂和伯仲胺(PSA)净化。在 BEH C UPLC 柱上进行 LC 分离,采用梯度洗脱,流动相由 0.5%甲酸(10 mM 乙酸铵)/甲醇组成。采用基质匹配的外标法定量,25 种农药在 0.5-100 μg/l 浓度范围内具有良好的线性关系,相关系数大于 0.9901。25 种农药的检出限(LOD)和定量限(LOQ)分别为 0.2-1.0 μg/kg 和 0.5-3.3 μg/kg。回收率在 72%-118%之间,相对标准偏差(RSD)小于 20%。因此,该方法适用于同时测定菰中 25 种农药。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/aff0/6624254/6483617002a8/41598_2019_46523_Fig1_HTML.jpg

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