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高效液相色谱-电感耦合等离子体质谱/质谱法测定大米中的草甘膦。

Determination of Glyphosate in White and Brown Rice with HPLC-ICP-MS/MS.

机构信息

Department for Sustainable Food Process, Università Cattolica del Sacro Cuore, Via Emilia Parmense 84, 29122 Piacenza, Italy.

出版信息

Molecules. 2022 Nov 19;27(22):8049. doi: 10.3390/molecules27228049.

Abstract

Background: In 2017, the European Commission renewed the approval of glyphosate (GLY) but only for five years. GLY remains one of the most controversial and studied molecules. Method: A simplified method was tested for the determination of GLY in white rice (WR) and brown rice (BR), after extraction only with a methanol solution, by liquid chromatography coupled with inductively coupled mass triple quadrupole (HPLC-ICP-MS/MS) with a PRP-X100 anionic column. After performing a test on groundwater, the quantification of GLY in WR and BR was validated in terms of the LOD, LOQ, accuracy, precision, linearity, and the matrix effect. Results: The LOD was 0.0027 mg kg−1 for WR and 0.0136 mg kg−1 for BR. The LOQ was 0.0092 mg kg−1 for WR and 0.0456 mg kg−1 for BR. The mean recoveries were within 76−105% at three fortification levels. The relative standard deviation for the analysis (five replicates for three spike levels) was < 11% for both matrices. A linear response was confirmed in all cases in the entire concentration range (R2WR = 1.000 and R2BR = 0.9818). Conclusion: The proposed method could be considered useful for the determination of GLY in different types of rice and designed and adapted for other cereals. The matrix effect, quantified in BR matrix extraction, could be avoided by using a matrix-matched calibration line.

摘要

背景

2017 年,欧盟委员会再次批准了草甘膦(GLY)的使用,但有效期仅为五年。GLY 仍然是最具争议和研究最多的分子之一。

方法

经过简化的方法,仅使用甲醇溶液提取,通过液相色谱-电感耦合等离子体质谱三重四极杆(HPLC-ICP-MS/MS)与 PRP-X100 阴离子柱,对糙米(BR)和白米(WR)中的 GLY 进行了检测。在对地下水进行测试后,根据 LOD、LOQ、准确度、精密度、线性和基质效应,对 WR 和 BR 中的 GLY 进行了定量验证。

结果

WR 的 LOD 为 0.0027 mg kg−1,BR 的 LOD 为 0.0136 mg kg−1。WR 的 LOQ 为 0.0092 mg kg−1,BR 的 LOQ 为 0.0456 mg kg−1。在三个加标水平下,平均回收率在 76-105%之间。两种基质的分析(三个加标水平的五个重复)的相对标准偏差均<11%。在所有情况下,整个浓度范围内均确认了线性响应(WR 的 R2 = 1.000,BR 的 R2 = 0.9818)。

结论

该方法可用于不同类型大米中 GLY 的测定,也可用于其他谷物。通过使用基质匹配校准线,可以避免 BR 基质提取中的基质效应。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/d2da/9696991/530a85fa7a85/molecules-27-08049-g001.jpg

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