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采用固相萃取-气相色谱-质谱联用技术同时测定人血清中的邻苯二甲酸酯和己二酸酯。

Simultaneous determination of phthalates and adipates in human serum using gas chromatography-mass spectrometry with solid-phase extraction.

作者信息

Guo Zhi-Yong, Gai Pan-Pan, Duan Jing, Zhai Jin-Xia, Zhao Sha-Sha, Wang Sui, Wei Dan-Yi

机构信息

Faculty of Materials Science and Chemical Engineering, The State Key Laboratory Base of Novel Functional Materials and Preparation Science, Ningbo University, Ningbo, Zhejiang 315211, PR China.

出版信息

Biomed Chromatogr. 2010 Oct;24(10):1094-9. doi: 10.1002/bmc.1410.

Abstract

A gas chromatography-mass spectrometry assay was developed and validated for the simultaneous determination of phthalates and adipates in human serum. The phthalates and adipates studied were dimethyl phthalate, diethyl phthalate, dibutyl phthalate, benzylbutyl phthalate, di-2-ethylhexyl phthalate, di-n-octyl phthalate, diethyl adipate, dibutyl adipate, diisobutyl adipate, bis(2-butoxyethyl) adipate and di-2-ethylhexyl adipate, with diisooctyl phthalate as internal standard. The extraction and cleaning up procedure was carried out with solid-phase extraction cartridges containing dimethyl butylamine groups, which showed extraction efficiencies over 88% for each analyte and the internal standard. The calibration curves obtained were linear with correlation coefficients greater than 0.98. For all analytes, the assay gave CV% values for intra-day precision from 4.9 to 13.3% and mean accuracy values from 91.4 to 108.4%, while inter-day precision was 5.2-13.4% and mean accuracy 91.0-110.2%. The limits of detection for the assay of phthalates and adipates were in the range 0.7-4.5 ng/mL. The method is simple, sensitive and accurate, and allows for simultaneous determination of nanogram levels of phthalates and adipates in human serum. It was successfully applied to an investigation on the level of phthalates and adipates in a non-occupationally exposed population.

摘要

建立并验证了一种气相色谱 - 质谱分析法,用于同时测定人血清中的邻苯二甲酸酯类和己二酸酯类。所研究的邻苯二甲酸酯类和己二酸酯类包括邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯、邻苯二甲酸苄基丁酯、邻苯二甲酸二(2 - 乙基己基)酯、邻苯二甲酸二正辛酯、己二酸二乙酯、己二酸二丁酯、己二酸二异丁酯、己二酸双(2 - 丁氧基乙基)酯和己二酸二(2 - 乙基己基)酯,以邻苯二甲酸二异辛酯作为内标。采用含有二甲基丁胺基团的固相萃取柱进行萃取和净化程序,每种分析物和内标的萃取效率均超过88%。得到的校准曲线呈线性,相关系数大于0.98。对于所有分析物,该分析方法日内精密度的CV%值为4.9%至13.3%,平均准确度值为91.4%至108.4%,而日间精密度为5.2% - 13.4%,平均准确度为91.0% - 110.2%。邻苯二甲酸酯类和己二酸酯类分析方法的检测限在0.7 - 4.5 ng/mL范围内。该方法简便、灵敏且准确,能够同时测定人血清中纳克水平的邻苯二甲酸酯类和己二酸酯类。它已成功应用于对非职业暴露人群中邻苯二甲酸酯类和己二酸酯类水平的调查。

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