Determination of 9 Organophosphorus Flame Retardants in Vegetables by High Performance Liquid Chromatography-Tandem Mass Spectrometry
摘 要
建立了测定蔬菜中9种有机磷阻燃剂的高效液相色谱-串联质谱法。采用QuEChERS法进行样品前处理,样品5.0 g经体积比4∶1的乙腈-丙酮混合液10 mL提取,除水,净化,氮吹至近干,以0.5 mL甲醇复溶后进样。以Waters ACQUITY UPLC® BEH C18色谱柱为固定相,以不同体积比的含0.1%(体积分数)甲酸的水溶液和含0.1%甲酸(体积分数)的甲醇溶液为流动相进行梯度洗脱分离,质谱分析采用电喷雾正离子源(ESI+)和多反应监测(MRM)模式,以离子对和保留时间定性,外标法定量。结果表明:9种有机磷阻燃剂的质量浓度在一定范围内呈线性关系,检出限(3S/N)为0.01~15 μg·kg-1。按标准加入法进行回收试验,测得回收率为60.0%~120%,测定值的相对标准偏差(n=5)均小于10%。按此方法分析了7种蔬菜样品,其中磷酸三乙酯(TEP)的检出率高达100%。
Abstract
A method for the determination of 9 organophosphorus flame retardants in vegetables was established by high performance liquid chromatography-tandem mass spectrometry. The QuEChERS method was used for sample pretreatment. The sample (5.0 g) was extracted with 10 mL of a mixture of acetonitrile and acetone at volume ratio of 4∶1, the water of which were removed, and the analytes were purified, blown to dryness by nitrogen and redissolved with 0.5 mL methanol. The chromatographic separation was performed by using Waters ACQUITY UPLC® BEH C18 chromatographic column as stationary phase, and the mixtures of aqueous solution containing 0.1% (φ) formic acid and methanol solution containing 0.1% (φ) formic acid at different volume ratios were used as mobile phase for gradient elution. ESI+ and the mode of multireaction monitoring (MRM) were adopted in MS/MS. Ion pair and retention time were used for qualitative analysis, and external standard method for quantitative analysis. The results showed that linear relationships of mass concentrations of 9 organophosphorus flame retardants were found in the definite ranges, with detection limits (3S/N) in the range of 0.01-15 μg·kg-1. Tests for recovery were made by standard addition method, giving results in the range of 60.0%-120%, and RSDs of the determined values (n=5) all less than 10%. This method was used to analyze the 7 Vegetable samples, and the detection rate of triethyl phosphate (TEP) was up to 100%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202106004
所属栏目 工作简报
基金项目 南京市医学科技发展项目(ZKX17048)
收稿日期 2020/5/20
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备注许珊珊,主要从事卫生理化检验工作
引用该论文: XU Shanshan,SUN Wenfang,YANG Wen,LIU Xiangping. Determination of 9 Organophosphorus Flame Retardants in Vegetables by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(6): 500~506
许珊珊,孙文芳,杨雯,刘祥萍. 高效液相色谱-串联质谱法测定蔬菜中9种有机磷阻燃剂的含量[J]. 理化检验-化学分册, 2021, 57(6): 500~506
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【7】郑春莉,冯珊珊,杜苗苗,等.固相微萃取/气相色谱-质谱联用技术在有机磷酸三酯阻燃剂土壤吸附分析中的应用[J].西安交通大学学报, 2015,49(11):128-134.
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