| 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 |
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| 基金项目:国家重点研发项目(2017YFC1600300） |
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| 中文摘要: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，1.7 μm）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0.005~100 μg/L范围内线性关系良好，检出限为0.002~0.030 μg/L，定量下限为0.005~0.100 μg/L，回收率为76.6%~122%，相对标准偏差(RSD）为060%~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。 |
| 中文关键词: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） |
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| Simultaneous Determination of 23 Bisphenol Analogs and Their Halogenated Derivatives in Urine and Serum by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry |
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| Abstract: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. |
| Key Words:bisphenol analogs and their halogenated derivatives urine serum pyridine 3 sulfonyl chloride ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS） |
| 引用本文：牛宇敏，王彬，杨润晖，段鹤君，张晶，邵兵.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[J].分析测试学报,2020,39(6):715-721. |
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