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Rapid and sensitive determination of nine bisphenol analogues, three amphenicol antibiotics, and six phthalate metabolites in human urine samples using UHPLC-MS/MS
Analytical and Bioanalytical Chemistry ( IF 4.3 ) Pub Date : 2018-04-19 , DOI: 10.1007/s00216-018-1062-2
Yuan Yao , Yijun Shao , Ming Zhan , Xiaoli Zou , Weidong Qu , Ying Zhou

Bisphenol analogues, amphenicol antibiotics, and phthalate have widely aroused public concerns due to their adverse effects on human health. In this study, a rapid and sensitive method for determination of nine bisphenol analogues, three amphenicol antibiotics, and six phthalate metabolites in the urine based on ultra-high-performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry was developed and validated. The sample pretreatment condition on the base of mixed-mode anion-exchange (Oasis MAX) SPE was optimized to separate bisphenol analogues and amphenicol antibiotics from phthalate metabolites: the former were detected with a mobile phase of 0.1% ammonium water solution/methanol containing 0.1% ammonium water solution in negative mode, whereas the latter were determined with a mobile phase of 0.1% acetic acid solution/acetonitrile containing 0.1% acetic acid in negative mode. The limits of detection were less than 0.26 ng/mL for bisphenol analogues, 0.12 ng/mL for amphenicol antibiotics, and 0.14 ng/mL for phathalate metabolites. The recoveries of all target analytes in three fortification levels ranged from 72.02 to 117.64% with the relative standard deviations of no larger than 14.51%. The matrix effect was adjusted by isotopically labeled internal standards. This proposed method was successfully applied to analyze 40 actual urines and 13 out of 18 studied compounds were detected.

中文翻译:

使用UHPLC-MS / MS快速灵敏地测定人尿液样品中的9种双酚类似物,3种苯甲酚类抗生素和6种邻苯二甲酸酯代谢物

双酚类似物,苯酚类抗生素和邻苯二甲酸酯由于其对人体健康的不利影响而引起了公众的广泛关注。在这项研究中,开发和验证了一种基于超高效液相色谱-三重四极杆串联质谱法测定尿液中的9种双酚类似物,3种苯酚类抗生素和6种邻苯二甲酸酯代谢物的快速灵敏方法。优化了基于混合模式阴离子交换(Oasis MAX)固相萃取的样品预处理条件,以从邻苯二甲酸酯代谢物中分离出双酚类似物和氨酚抗生素:流动相为0.1%铵水溶液/甲醇(含0.1)负模态的铵水溶液,而后者的流动相为0。1%的乙酸溶液/乙腈,以负模方式包含0.1%的乙酸。双酚类似物的检出限小于0.26 ng / mL,氨苄青霉素抗生素的检出限小于0.12 ng / mL,邻苯二甲酸酯代谢物的检出限小于0.12 ng / mL。三种设防水平下所有目标分析物的回收率在72.02%至117.64%之间,相对标准偏差不大于14.51%。基质效应通过同位素标记的内标进行调整。该建议方法已成功应用于分析40种实际尿液,并检测出18种研究化合物中的13种。三种设防水平下所有目标分析物的回收率在72.02%至117.64%之间,相对标准偏差不大于14.51%。基质效应通过同位素标记的内标进行调整。该建议方法已成功应用于分析40种实际尿液,并检测出18种研究化合物中的13种。三种设防水平下所有目标分析物的回收率在72.02%至117.64%之间,相对标准偏差不大于14.51%。基质效应通过同位素标记的内标进行调整。该建议方法已成功应用于分析40种实际尿液,并检测出18种研究化合物中的13种。
更新日期:2018-04-19
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