超高效液相色谱-串联质谱法测定尿液中4种环己烷1,2-二甲酸二异壬基酯增塑剂代谢物

引用本文: 韩林学, 邱天, 林潇, 刘嘉融, 胡小键, 张续. 超高效液相色谱-串联质谱法测定尿液中4种环己烷1,2-二甲酸二异壬基酯增塑剂代谢物[J]. 分析化学, 2023, 51(2): 229-238. doi: 10.19756/j.issn.0253-3820.221183 shu

Citation: HAN Lin-Xue, QIU Tian, LIN Xiao, LIU Jia-Rong, HU Xiao-Jian, ZHANG Xu. Determination of Four Metabolites of Di(isononyl) Cyclohexane-1,2-dicarboxylate in Urine via Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2023, 51(2): 229-238. doi: 10.19756/j.issn.0253-3820.221183 shu

超高效液相色谱-串联质谱法测定尿液中4种环己烷1,2-二甲酸二异壬基酯增塑剂代谢物

韩林学 ^1, ,
邱天 ^1, ,
林潇 ^1, ,
刘嘉融 ^2, ,
胡小键 ^1, ,
张续 ^{1,
,}

1.
中国疾病预防控制中心环境与健康相关产品安全所, 环境与人群健康重点实验室, 北京 100021;
2.
首都医科大学燕京医学院, 北京 101300

通讯作者: 张续,E-mail:zhangxu@nieh.chinacdc.cn

基金项目:
国家自然科学基金项目(No.22106154)、环境化学与生态毒理学国家重点实验室开放基金项目(No.KF2020-17)和持久性有毒污染物环境与健康危害湖北省重点实验室开放基金项目(No.PTS2019-08)资助。

摘要: 建立了尿液中4种环己烷1,2-二甲酸二异壬基酯（DINCH）增塑剂代谢物的超高效液相色谱-串联质谱测定方法。2 mL尿液经β-葡萄糖醛酸酶/芳基硫酸酯酶水解，采用阴离子交换固相萃取柱对目标分析物进行富集净化，氮吹浓缩至0.5 mL。以Acquity BEH C₁₈色谱柱（100 mm×2.1 mm，1.7 μm）作为分析柱，0.05%乙酸乙腈和0.05%乙酸作为流动相进行梯度洗脱，在电喷雾负电离多反应监测模式下进行定性和内标法定量分析。4种DINCH代谢物在0.01~50 ng/mL浓度范围内线性关系良好，相关系数（r）大于0.9996，方法检出限为0.01~0.03 ng/mL，方法定量限为0.03~0.10 ng/mL，加标回收率为74%~124%，相对标准偏差为1.2%~15.0%，日内精密度为3.5%~6.2%，日间精密度为6.9%~9.8%。应用此方法测定了55份尿液样本，结果显示，4种DINCH代谢物均可检出。MINCH、oxo-MINCH、OH-MINCH和cx-MINCH的检出率分别为18.2%、47.3%、98.2%和100%，检出浓度分别为

关键词:

English

Determination of Four Metabolites of Di(isononyl) Cyclohexane-1,2-dicarboxylate in Urine via Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

1.
China CDC Key Laboratory of Environment and Population Health, National Institute of Environmental Health, Chinese Center for Disease Control and Prevention, Beijing 100021, China;
2.
Yanjing Medical College, Capital Medical University, Beijing 101300, China

Corresponding author: ZHANG Xu, zhangxu@nieh.chinacdc.cn

Received Date: 15 April 2022
Revised Date: 19 October 2022
Fund Project:
Supported by the National Natural Science Foundation of China (No. 22106154), the State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences (No. KF2020-17) and the Project of Hubei Key Laboratory of Environmental and Health Effects of Persistent Toxic Substances (No. PTS2019-08).

Abstract: A method for quantification of four kinds of metabolites of di(isononyl) cyclohexane-1,2-dicarboxylate (DINCH) in urine using ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed. Urine sample (2 mL) were deconjugated by β-glucuronidase/arylsulfatase, extracted and cleaned using anion-exchange solid phase extraction cartridge and concentrated to 0.5 mL under gentle stream of nitrogen. The target analytes were separated on Waters Acquity UPLC BEH C₁₈ Column (100 mm×2.1 mm,1.7 μm), and eluted with 0.05% (V/V) acetic acid in water and 0.05% (V/V) acetic acid in acetonitrile in gradient. The target analytes were ionized in negative electrospray ionization (ESI-) mode and scanned under a multiple reaction monitoring (MRM) mode. Quantitative analysis of target analytes in urine was achieved by isotope labelled standard assay. In the range of 0.01-50 ng/mL, all four target analytes exhibited good linearity with correlation coefficients (r) above 0.9996. The method detection limits (MDLs) and method quantification limits (MQLs) were 0.01-0.03 ng/mL and 0.03-0.10 ng/mL, respectively. The recoveies were from 74% to 124%, with the relative standard deviations (RSD) between 1.2% and 15.0%. The intra-day and inter-day precisions were 3.5%-6.2% and 6.9%-9.8%, respectively. The developed method was performed to determinate the DINCH metabolites in 55 human urine samples collected in Beijing. All four DINCH metabolites were detected in urine, and the detected rates of MINCH, oxo-MINCH, OH-MINCH and cx-MINCH were 18.2%, 47.3%, 98.2% and 100%, respectively. The four metabolites were detected in the concentration ranges of

Key words:

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超高效液相色谱-串联质谱法测定尿液中4种环己烷1,2-二甲酸二异壬基酯增塑剂代谢物

通讯作者: 张续,E-mail:zhangxu@nieh.chinacdc.cn

English

Determination of Four Metabolites of Di(isononyl) Cyclohexane-1,2-dicarboxylate in Urine via Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

Corresponding author: ZHANG Xu, zhangxu@nieh.chinacdc.cn

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超高效液相色谱-串联质谱法测定尿液中4种环己烷1,2-二甲酸二异壬基酯增塑剂代谢物

通讯作者: 张续,E-mail:zhangxu@nieh.chinacdc.cn

English

Determination of Four Metabolites of Di(isononyl) Cyclohexane-1,2-dicarboxylate in Urine via Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

Corresponding author: ZHANG Xu, zhangxu@nieh.chinacdc.cn

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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