方法用液相色谱-质谱法测定玉米和土壤中吡虫啉及其代谢物的方法验证。

IF 1.5 4区 化学 Q4 BIOCHEMICAL RESEARCH METHODS
Sandeep Kaur, Smriti Sharma, Balpreet K Kang
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引用次数: 0

摘要

采用液相色谱串联质谱联用电喷雾电离法对玉米叶片、未熟籽粒、成熟籽粒、秸秆和土壤中吡虫啉(IM)及其代谢物进行了快速、简便、廉价、有效、可靠和安全(QuEChERS)方法的验证。用乙腈+0.1%甲酸在玉米和土壤的不同基质中进行提取,然后用伯仲胺吸附剂和无水硫酸镁进行清理。从选择性、线性、检出限、定量限、基质效应、离子比、质量控制、鲁棒性、准确度和精密度等方面对方法进行了验证。所有参数的验证都是按照欧洲委员会卫生和食品安全总局(DG SANTE)的指导方针进行的。溶剂与不同基质(玉米叶片、未熟籽粒、成熟籽粒、秸秆、土壤)呈线性关系,相关系数R2 > 0.99。回收率为78%,相对标准偏差为小于5.4%。该方法简便、灵敏、准确、经济、精确、快速地从玉米叶片、未成熟籽粒、成熟籽粒、秸秆和土壤中提取IM及其代谢物。这可以帮助残留分析人员解决有效的残留估计,定期监测残留,也可以帮助在玉米中使用IM的监管和食品安全问题。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Method Validation for Estimation of Imidacloprid and its Metabolites in Maize and Soil by LCMS-MS.

Validation of Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) method was performed for estimation of imidacloprid (IM) and its metabolites in maize leaves, immature kernels, mature kernels, stalk, and soil using liquid chromatograph tandem mass spectrometry, coupled with electrospray ionization. The extraction in different matrices of maize and soil was performed using acetonitrile +0.1% formic acid followed by clean-up with primary secondary amine sorbent and anhydrous magnesium sulfate. The method was validated in terms of selectivity, linearity, limit of detection, limit of quantification, matrix effect, ion ratios, quality control, robustness, accuracy, and precision. The validation of all parameters was done in accordance with European Commission's Directorate-General for Health and Food Safety (DG SANTE) guidelines. A linear relationship with high correlation coefficients R2 > 0.99 was obtained for solvents and different matrices viz., maize leaves, immature kernels, mature kernels, stalk, and soil. The recovery and relative standard deviations were ˃78% and ˂5.4%, respectively. This method permits a simple, sensitive, accurate, cost-effective, precise, and rapid extraction of IM and its metabolites from maize leaves, immature kernels, mature kernels, stalks, and soil. This can help the residue analysts to address effective residue estimation, regular monitoring of residues and can also aid in the regulatory and food safety concerns about the usage of IM in maize.

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来源期刊
CiteScore
2.90
自引率
7.70%
发文量
94
审稿时长
5.6 months
期刊介绍: The Journal of Chromatographic Science is devoted to the dissemination of information concerning all methods of chromatographic analysis. The standard manuscript is a description of recent original research that covers any or all phases of a specific separation problem, principle, or method. Manuscripts which have a high degree of novelty and fundamental significance to the field of separation science are particularly encouraged. It is expected the authors will clearly state in the Introduction how their method compares in some markedly new and improved way to previous published related methods. Analytical performance characteristics of new methods including sensitivity, tested limits of detection or quantification, accuracy, precision, and specificity should be provided. Manuscripts which describe a straightforward extension of a known analytical method or an application to a previously analyzed and/or uncomplicated sample matrix will not normally be reviewed favorably. Manuscripts in which mass spectrometry is the dominant analytical method and chromatography is of marked secondary importance may be declined.
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