超高效液相色谱-串联质谱法同时测定尿液与血清中23种双酚类化合物  

Simultaneous Determination of 23 Bisphenol Analogs and Their Halogenated Derivatives in Urine and Serum by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：牛宇敏[1] 王彬 杨润晖 段鹤君[1] 张晶[1] 邵兵[1] NIU Yu-min;WANG Bin;YANG Run-hui;DUAN He-jun;ZHANG Jing;SHAO Bing(Beijing Key Laboratory of Diagnostic and Traceability Technologies for Food Poisoning,Beijing Center for Disease Prevention and Control,Beijing 100013,China;Chinese Academy of Inspection and Quarantine Comprehensive Test Center,Beijing 100123,China;College of Food Engineering and Biotechnology,Tianjin University of Science&Technology,Tianjin 300457,China)

机构地区：[1]北京市疾病预防控制中心食物中毒诊断溯源技术北京市重点实验室,北京100013 [2]中国检验检疫科学研究院综合检测中心,北京100123 [3]天津科技大学食品工程与生物技术学院,天津300457

出　　处：《分析测试学报》2020年第6期715-721,共7页Journal of Instrumental Analysis

基　　金：国家重点研发项目(2017YFC1600300)。

摘　　要：建立了基于吡啶-3-磺酰氯衍生和超高效液相色谱-串联质谱(UPLC-MS/MS)检测尿液和血清中23种双酚类化合物(BPs)的方法。尿液样品采用乙酸乙酯提取;血清样品采用乙腈提取,上清液经PRiME HLB柱净化。提取液经吡啶-3-磺酰氯衍生后,以乙腈和0.1%甲酸水溶液为流动相,采用ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7μm)色谱柱进行分离。质谱离子源为电喷雾电离源,正离子模式检测。23种目标物在0.005~100μg/L范围内线性关系良好,检出限为0.002~0.030μg/L,定量下限为0.005~0.100μg/L,回收率为76.6%~122%,相对标准偏差(RSD)为0.60%~14%。使用建立的方法分别对20份尿液和20份血清样品进行了检测。该方法样品用量少,灵敏度高,可以满足尿液和血清样品中23种BPs的同时测定要求。An ultra-high performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for the simultaneous determination of 23 bisphenol analogs and their halogenated derivatives(BPs) in urine and serum based on derivatization of pyridine-3-sulfonyl chloride.Urine samples were extracted by liquid-liquid extraction with ethyl acetate,while serum samples were extracted with acetonitrile and followed by PRiME HLB cartridge purification.After derivatization with pyridine-3-sulfonyl chloride,the extracts were separated on an ACQUITY UPLC BEH C18(2.1 mm×100 mm,1.7 μm) column with acetonitrile and water containing 0.1% formic acid as mobile phases,and determined by UPLC-MS/MS with electrospray ionization(ESI) in positive ion mode.There were good linear relationships for 23 BPs in both urine and serum samples in the range of 0.005-100 μg/L,with their limits of detection between 0.002 μg/L and 0.030 μg/L,limits of quantitation between 0.005 μg/L and 0.100 μg/L.Average recoveries ranged from 76.6% to 122%,with relative standard deviations(RSD) of 0.60%-14%.The method was applied in the analysis of BPs in 20 urine samples and 20 serum samples.The method could meet the requirements for simultaneous determination of 23 BPs in urine and serum samples with low sample consumption and high sensitivity.

关 键 词：双酚类化合物 尿液 血清 吡啶-3-磺酰氯 超高效液相色谱-串联质谱(UPLC-MS/MS) 

分 类 号：O657.63[理学—分析化学] O657.7[理学—化学]