Department of Clinical Sciences and Community Health, Università degli Studi di Milano, Milan, Italy.
Environmental and Industrial Toxicology Unit, Fondazione IRCCS Ca' Granda Ospedale Maggiore Policlinico, Milan, Italy.
Rapid Commun Mass Spectrom. 2020 Jul 15;34(13):e8796. doi: 10.1002/rcm.8796.
Several phthalates and bisphenol A are endocrine-disrupting chemicals (EDCs). Recently, their use has been partially restricted and less toxic compounds, such as di-2-ethylhexyl terephthalate (DEHTP), have been placed on the market. The aim of this work was to develop and validate a method for the simultaneous quantitation of bisphenol A and urinary metabolites of phthalates, including DEHTP.
An isotopic dilution high-performance liquid chromatography/electrospray ionization tandem mass spectrometry (HPLC/ESI-MS/MS) method for the determination of bisphenol A (BPA), monobenzyl phthalate (MBzP), mono-2-ethyl-5-carboxypentyl phthalate (MECPP), mono-2-ethyl-5-carboxypentyl terephthalate (MECPTP), mono-2-ethyl-5-hydroxyhexyl terephthalate (MEHHTP), monoethyl phthalate (MEP), and mono-n/i-butyl phthalates (MnBP/MiBP) in human urine was developed. A complete validation was carried out and the method was applied to 36 non-occupationally exposed adults.
Limits of quantitation ranged from 0.02 (MECPP) to 1 μg/L (MnBP and MiBP). Relative standard deviations below 10% indicated a suitable precision; accuracy, evaluated using a standard reference material, ranged from 74.3% to 117.5%; isotopically labelled internal standards were suitable for correcting the matrix effect. The accuracy was confirmed by the successful participation in an external verification exercise. However, for terephthalates, the validation was incomplete due to the lack of reference materials and external verification. Levels of the investigated chemicals in subjects were in line with those previously reported.
An LC/MS/MS assay for the simultaneous measurement of BPA and phthalate metabolites in human urine was developed and validated; it is useful to investigate exposure in epidemiological studies involving the general population.
邻苯二甲酸酯和双酚 A 是几种内分泌干扰化学物质（EDCs）。最近，它们的使用受到了一定限制，市场上出现了毒性较低的化合物，如邻苯二甲酸二（2-乙基己基）酯（DEHTP）。本研究旨在开发和验证一种同时定量测定双酚 A 和邻苯二甲酸酯尿液代谢物的方法，包括 DEHTP。
建立了一种同位素稀释高效液相色谱/电喷雾串联质谱（HPLC/ESI-MS/MS）法，用于测定尿液中双酚 A（BPA）、单苄基邻苯二甲酸酯（MBzP）、单-2-乙基-5-羧基戊基邻苯二甲酸酯（MECPP）、单-2-乙基-5-羧基戊基邻苯二甲酸酯（MECPTP）、单-2-乙基-5-羟己基邻苯二甲酸酯（MEHHTP）、邻苯二甲酸单乙酯（MEP）和邻苯二甲酸单正丁基和单异丁基酯（MnBP/MiBP）。对该方法进行了全面验证，并应用于 36 名非职业暴露的成年人。
定量下限范围为 0.02（MECPP）至 1μg/L（MnBP 和 MiBP）。相对标准偏差低于 10%表明精密度良好；用标准参考物质评估的准确度范围为 74.3%至 117.5%；同位素标记的内标适用于校正基质效应。通过成功参与外部验证活动，确认了准确度。然而，由于缺乏参考物质和外部验证，邻苯二甲酸酯的验证并不完整。研究对象中所研究化学物质的水平与先前报道的水平一致。
本研究开发并验证了一种同时测定人尿液中 BPA 和邻苯二甲酸酯代谢物的 LC/MS/MS 检测方法；该方法可用于研究一般人群的流行病学研究中的暴露情况。
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