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加速溶剂萃取-QuEChERS/超高效液相色谱-串联质谱法同时测定药食同源性食品中双酚类化合物
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作者单位
曾静,曲栗,古淑青,邓晓军,伊雄海,张晶,丁涛,柳菡 1.上海海关动植物与食品检验检疫技术中心2.复旦大学公共卫生学院3.北京市疾病预防控制中心4.南京海关动植物与食品检测中心 
基金项目:国家重点研发计划项目(2017YFF0211003);上海市技术标准专项项目(18DZ2201100);海关总署科研项目(2019HK099)
中文摘要:建立了加速溶剂萃取(ASE)-QuEChERS/超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定药食同源性食品中11种双酚类化合物残留的分析方法。样品经ASE萃取,萃取溶剂为乙腈-乙酸-水(89∶1∶10,体积比),萃取温度为80 ℃,静态萃取时间为6 min,循环2次。萃取液经QuEChERS法净化,采用ACQUITY UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8 μm)分离,以甲醇(含0.1%甲酸)和5 mmol/L乙酸铵水溶液(含0.1%甲酸)为流动相进行梯度洗脱,电喷雾电离源正、负模式下同时进行多反应监测(MRM)测定,同位素内标法定量。11种双酚类化合物在0.5~50.0 μg/L范围内呈良好线性,相关系数(r2)不小于0.996 0,检出限为0.1~0.5 μg/kg,定量下限为0.3~1.5 μg/kg;3个加标水平的回收率为72.4%~108%,相对标准偏差(RSD)为1.7%~15%。该方法操作简单、快速、灵敏度高、重现性好,适用于药食同源性食品中双酚类化合物的同时快速测定。
中文关键词:加速溶剂萃取(ASE)  QuEChERS  超高效液相色谱-串联质谱(UPLC-MS/MS)  双酚类化合物  药食同源
 
Determination of Bisphenol Substances in Drug and Food Homologous Products by Ultra-performance Liquid Chromatography-Tandem Mass Spectrometry Combined with Accelerated Solvent Extraction and QuEChERS
Abstract:A method was developed for the simultaneous determination of bisphenol substances in drug and food homologous products by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) combined with accelerated solvent extraction(ASE) and QuEChERS.The samples were extracted at 80 ℃ via two cycles of ASE,with acetonitrile-acetic acid-water(89∶1∶10,by volume) for 6 min,then purified by QuEChERS.11 bisphenol substances were separated on an ACQUITY UPLC HSS T3 column(2.1 mm×100 mm,1.8 μm) by gradient elution using methanol containing 0.1% formic acid and 5 mmol/L ammonium acetate containing 0.1% formic acid as mobile phases,then analyzed by MS/MS with electrospray ionization in positive and negative mode under multiple reaction monitoring(MRM) mode,finally quantified by internal standard method.There were good linear relationships for 11 bisphenol substances in the concentration range of 0.5-50.0 μg/L,with correlation coefficients(r2) not less than 0.996 0.The limits of detection(LOD) and limits of quantitation(LOQ) for 11 bisphenol substances were in the ranges of 0.1-0.5 μg/kg and 0.3-1.5 μg/kg,respectively.The recoveries at three spiked levels ranged from 72.4% to 108% with relative standard deviations(RSD) of 1.7%-15%.The proposed method was simple,rapid,high sensitive and reproducible,and it was suitable for the rapid determination of 11 bisphenol substances in drug and food homologous products.
Key Words:accelerated solvent extraction(ASE)  QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  bisphenol substances  drug and food homologous products
引用本文:曾静,曲栗,古淑青,邓晓军,伊雄海,张晶,丁涛,柳菡.加速溶剂萃取-QuEChERS/超高效液相色谱-串联质谱法同时测定药食同源性食品中双酚类化合物[J].分析测试学报,2020,39(6):736-742.
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