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基质固相分散结合气相色谱-串联质谱法同时测定蔬菜中 13 种有机磷酯。

Matrix solid-phase dispersion coupled with gas chromatography-tandem mass spectrometry for simultaneous determination of 13 organophosphate esters in vegetables.

机构信息

Key Laboratory of Regional Environment and Eco-Remediation of Ministry of Education, College of Environment, Shenyang University, Shenyang, 110044, Liaoning, China.

出版信息

Anal Bioanal Chem. 2018 Nov;410(27):7077-7084. doi: 10.1007/s00216-018-1308-z. Epub 2018 Aug 28.

DOI:10.1007/s00216-018-1308-z
PMID:30155700
Abstract

In this study, matrix solid-phase dispersion coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the analysis of 23 organophosphate esters (OPEs) in vegetables. Under the optimal conditions, 0.5 g vegetables was dispersed with use of 2 g Florisil, 2 g anhydrous sodium sulfate, and 0.1 g graphitized carbon black, and it was transferred to an empty solid-phase extraction cartridge. The analytes were eluted with 15 mL n-hexane/acetone (1:1, v/v) and analyzed by GC-MS/MS. The method detection limits and quantitation limits ranged from 0.05 to 0.33 ng/g and from 0.16 to 1.10 ng/g, respectively. The recoveries ranged from 65.1% to 109.1%, and the relative standard deviations were less than 15%. The analysis of eight kinds of vegetables shows that the vegetables had been contaminated by OPEs; the concentrations of the sum of the OPEs ranged from 5.89 to 26.8 ng/g. The proposed method is applicable to analyze OPEs in vegetables. Graphical abstract ᅟ.

摘要

在这项研究中,建立了基质固相分散结合气相色谱-串联质谱法(GC-MS/MS)用于分析蔬菜中的 23 种有机磷酸酯(OPEs)。在最佳条件下,用 2 g Florisil、2 g 无水硫酸钠和 0.1 g 石墨化炭黑分散 0.5 g 蔬菜,并将其转移到空固相萃取小柱中。用 15 mL 正己烷/丙酮(1:1,v/v)洗脱分析物,并用 GC-MS/MS 分析。方法检出限和定量限范围分别为 0.05-0.33ng/g 和 0.16-1.10ng/g。回收率范围为 65.1%-109.1%,相对标准偏差小于 15%。对 8 种蔬菜的分析表明,蔬菜已被 OPEs 污染;OPEs 的总和浓度范围为 5.89-26.8ng/g。所提出的方法适用于分析蔬菜中的 OPEs。

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