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高效薄层色谱法结合 HPLC-DAD/HPLC-MS/MS 用于同时测定生物样品中双酚 A 和九种溴代类似物。

High-performance thin-layer chromatography coupled with HPLC-DAD/HPLC-MS/MS for simultaneous determination of bisphenol A and nine brominated analogs in biological samples.

机构信息

CAS Key Laboratory of Biobased Materials, Qingdao Institute of Bioenergy and Bioprocess Technology, Chinese Academy of Sciences, Qingdao, 266101, Shandong, China.

Research Center for Analytical Sciences, College of Sciences, Northeastern University, Shenyang, 110819, Liaoning, China.

出版信息

Anal Bioanal Chem. 2019 Jan;411(3):725-734. doi: 10.1007/s00216-018-1492-x. Epub 2018 Dec 1.

DOI:10.1007/s00216-018-1492-x
PMID:30506505
Abstract

Bisphenol A (BPA) and its brominated analogs exhibiting bioaccumulation potential, endocrine disruption, and reproductive toxicity have been worldwide detected in water, air, soil, and sediments. But few methods have been proposed for simultaneously determining a variety of these compounds in biological matrices, hindering the further study on their biological transformation/degradation and health risks. In this study, a simple, solvent-saving and sensitive method based on high-performance thin-layer chromatography (HPTLC) for sample pretreatment coupled with high-performance liquid chromatography-diode array detector (HPLC-DAD) (UV = 214 nm)/triple quadrupole mass spectrometry (MS/MS) was developed for determining BPA and its nine brominated analogs in biological samples. The method detection limits (MDLs) and method quantification limits (MQLs) for ten BPA analogs ranged from 0.8 to 685.7 ng g dw (S/N = 3) and 2.7 to 2285.7 ng g dw (S/N = 10), respectively. The recoveries were 64-124% with SD less than 10%. The RSD of intermediate precision was less than 11%, and matrix effects were lower than 19%. Compared with traditional purification procedures, HPTLC largely reduced the workload and procedures for complex biological sample cleanup without inducing decomposition of the analytes. The proposed method exhibited good performance when detecting these ten chemicals in chicken samples from a nearby yard of brominated flame retardant plants, indicating its great potential for investigating their environment level, behavior, and fate in organisms. Graphical abstract ᅟ.

摘要

双酚 A(BPA)及其具有生物蓄积潜力、内分泌干扰和生殖毒性的溴代类似物已在世界各地的水、空气、土壤和沉积物中被检测到。但是,很少有方法被提出用于同时测定生物基质中多种此类化合物,这阻碍了对其生物转化/降解和健康风险的进一步研究。在本研究中,开发了一种基于高效薄层色谱(HPTLC)的简单、节省溶剂且灵敏的样品预处理方法,结合高效液相色谱-二极管阵列检测器(HPLC-DAD)(UV=214nm)/三重四极杆质谱(MS/MS),用于测定生物样品中的 BPA 及其九种溴代类似物。十种 BPA 类似物的方法检测限(MDL)和方法定量限(MQL)范围为 0.8 至 685.7ngg dw(S/N=3)和 2.7 至 2285.7ngg dw(S/N=10)。回收率为 64-124%,SD 小于 10%。中间精密度的 RSD 小于 11%,基质效应低于 19%。与传统的净化程序相比,HPTLC 大大减少了复杂生物样品净化的工作量和程序,而不会引起分析物的分解。当在来自附近溴化阻燃剂工厂的鸡样品中检测这十种化学物质时,该方法表现出良好的性能,表明其在调查这些化学物质在环境中的水平、行为和命运方面具有很大的潜力。

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