A modified method for the simultaneous determination of fluindapyr and its metabolites residues in vegetables and fruits by SPE and UHPLCMS/MS

IF 4 2区 农林科学 Q2 CHEMISTRY, APPLIED
Wei Han , Hongxia Tang , Li Zhao , Yubo Li , Dianying Men , Maofeng Dong , Lijun Han , Weimin Wang
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Abstract

A sensitive and reliable method for the determination of fluindapyr residue and its five metabolites is necessary in its registration, application and dissipation researches. Two typical national standard multi-residue analytical methods that involved fluindapyr was validated in this study, and the results found that both the methods gave low recoveries for one or more analytes and were not satisfied for detecting the residues of fluindapyr and its metabolites simultaneously. With comprehensive optimization, a simple and efficient method was established using mixed solution extraction with acetonitrile and water and cleaning-up by a modified SPE procedure with mixed-mode cation exchange cartridges, followed by ultrahigh-performance liquid chromatographytandem mass spectrometry (UHPLCMS/MS) detection for the simultaneous determination of fluindapyr and its five metabolites in vegetables and fruits. Method validation in nine vegetables and fruits was performed by analyzing the linearity (0.001–0.5 mg/L, and R2 ≥ 0.99), matrix effects (−95 %–80 %), fortified recoveries (71 %–118 %), relative standard deviations (0.2 %–16 %), limits of detection (0.0001–0.0002 mg/L), limits of quantification (0.0003–0.0006 mg/L) and the method limits of quantification (0.001 mg/kg). The proposed method was highly sensitive and reliable, and provides beneficial supplement to the two national standards in China in the simultaneously analysis of fluindapyr and its five metabolites in vegetables and fruits, and this study also provides reference for the method establishment for highly water-soluble analytes.
采用 SPE 和 UHPLCMS/MS 同时测定蔬菜和水果中氟啶虫酰胺及其代谢物残留的改进方法
在氟草胺的登记、应用和消散研究中,需要一种灵敏可靠的方法来测定氟草胺及其五种代谢物的残留量。本研究对两种典型的涉及氟啶虫酰胺的国家标准多残留分析方法进行了验证,结果发现这两种方法对一种或多种被分析物的回收率均较低,不能满足同时检测氟啶虫酰胺及其代谢物残留的要求。经过综合优化,建立了一种简便、高效的方法,采用乙腈-水混合溶液萃取,混合模式阳离子交换柱SPE净化,超高效液相色谱-串联质谱(UHPLCMS/MS)检测,可同时测定蔬菜和水果中氟啶虫酰胺及其5种代谢物的残留量。通过分析线性关系(0.001-0.5 mg/L,R2≥0.99)、基质效应(-95 %-80 %)、加标回收率(71 %-118 %)、相对标准偏差(0.2 %-16 %)、检出限(0.0001-0.0002 mg/L)、定量限(0.0003-0.0006 mg/L)和方法定量限(0.001 mg/kg),对 9 种蔬菜和水果中的方法进行了验证。该方法灵敏度高、可靠性好,为同时分析蔬菜和水果中氟啶虫酰胺及其5种代谢物提供了两个国家标准的有益补充,同时也为高水溶性分析物的方法建立提供了参考。
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来源期刊
Journal of Food Composition and Analysis
Journal of Food Composition and Analysis 工程技术-食品科技
CiteScore
6.20
自引率
11.60%
发文量
601
审稿时长
53 days
期刊介绍: The Journal of Food Composition and Analysis publishes manuscripts on scientific aspects of data on the chemical composition of human foods, with particular emphasis on actual data on composition of foods; analytical methods; studies on the manipulation, storage, distribution and use of food composition data; and studies on the statistics, use and distribution of such data and data systems. The Journal''s basis is nutrient composition, with increasing emphasis on bioactive non-nutrient and anti-nutrient components. Papers must provide sufficient description of the food samples, analytical methods, quality control procedures and statistical treatments of the data to permit the end users of the food composition data to evaluate the appropriateness of such data in their projects. The Journal does not publish papers on: microbiological compounds; sensory quality; aromatics/volatiles in food and wine; essential oils; organoleptic characteristics of food; physical properties; or clinical papers and pharmacology-related papers.
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