Determination of 12 Metabolites of Phthalates in Urine by High Performance Liquid Chromatography- Tandem Mass Spectrometry
摘 要
在2 mL尿液样品中加入4 mg·L-1混合内标溶液0.01 mL、不低于850 U·mL-1的β-葡萄糖醛酸酶溶液和1 mol·L-1乙酸铵溶液0.5 mL,充分振荡后于37℃水解2.0 h,降至室温,用乙腈定容至5 mL,冷冻2 h,恢复至常温后,过0.22 μm有机滤膜。采用高效液相色谱-串联质谱法同时测定其中12种邻苯二甲酸酯类代谢物的含量,基质匹配法消除基质干扰,内标法定量。结果表明,12种邻苯二甲酸酯类代谢物工作曲线的线性范围均为1.00~200 μg·L-1,检出限(3S/N)为0.05~1.88 μg·L-1。按标准加入法进行回收试验,回收率为75.3%~114%,测定值的相对标准偏差(n=6)为1.5%~10%。方法用于测定35份儿童尿液样品,其中检出11种邻苯二甲酸酯类代谢物,邻苯二甲酸单异癸酯(MDP)未检出。
Abstract
The mixed internal standard solution (4 mg·L-1, 0.01 mL), β-glucuronidase solution not less than 850 U·mL-1 and 0.5 mL of 1 mol·L-1 ammonium acetate solution were added into 2 mL of the urine sample. After shaking fully, the mixture was hydrolyzed at 37℃ for 2.0 h. After cooling to the room temperature, the volume of the solution was made up to 5 mL with acetonitrile. The solution was froze for 2 h, warmed to the room temperature, and filtered through 0.22 μm organic filter membrane. The 12 metabolites of phthalates in the above solution were determined by high performance liquid chromatography-tandem mass spectrometry, using matrix matching method to eliminate the matrix interference, and internal standard method to quantify. As shown by the results, the linear ranges of working curves of 12 metabolites of phthalates were all 1.00-200 μg·L-1, with detection limits (3S/N) in the range of 0.05-1.88 μg·L-1. Test for recovery was made by standard addition method, giving results in the range of 75.3%-114%, with RSDs (n=6) of the determined values in the range of 1.5%-10%. This method was applied to determination of 35 children urine samples, of which 11 metabolites of phthalates were detected, and monoisodecyl phthalate (MDP) was not detected.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202206015
所属栏目 工作简报
基金项目 2020年常州市卫健委青年人才科技项目(QN202051)
收稿日期 2021/10/16
修改稿日期
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联系人作者黎俊宏(37355396@qq.com)
备注石飞云,高级实验师,从事色谱和质谱应用研究工作
引用该论文: SHI Feiyun,XU Mengyuan,JIN Yi,TANG Hongbing,OUYANG Yunfu,LI Junhong. Determination of 12 Metabolites of Phthalates in Urine by High Performance Liquid Chromatography- Tandem Mass Spectrometry[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2022, 58(6): 708~714
石飞云,徐梦媛,靳艺,唐宏兵,欧阳运富,黎俊宏. 高效液相色谱-串联质谱法同时测定尿液中12种邻苯二甲酸酯类代谢物的含量[J]. 理化检验-化学分册, 2022, 58(6): 708~714
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参考文献
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【2】WENZEL A G, BROCK J W, CRUZE L, et al. Prevalence and predictors of phthalate exposure in pregnant women in Charleston, SC.[J] Chemosphere, 2018,193:394-402.
【3】林兴桃.邻苯二甲酸酯及其代谢物分析方法研究及暴露评价[D].北京:北京工业大学, 2012.
【4】张梅如,邱竞逸,王蕾,等.上海市152对乳母婴儿尿中邻苯二甲酸酯累积暴露的风险评估[J].卫生研究, 2017,46(2):237-243.
【5】WANG Y, ZHU H K, KANNAN K. A review of biomonitoring of phthalate exposures[J]. Toxics, 2019,7(2):21-21.
【6】KATSIKANTAMI I, TZATZARAKIS M N, ALEGAKIS A K, et al. Phthalate metabolites concentrations in amniotic fluid and maternal urine:Cumulative exposure and risk assessment[J]. Toxicology Reports, 2020,7:529-538.
【7】DU Y K, SAHO C, YERIN J, et al. Phthalate plasticizers in children's products and estimation of exposure:Importance of migration rate[J]. International Journal of Environmental Research and Public Health, 2020,17(22):8582.
【8】JEONG J Y, LEE J H, KIM E Y, et al. Determination of phthalate metabolites in human serum and urine as biomarkers for phthalate exposure using column-switching LC-MS/MS[J]. Safety and Health at Work, 2011,2(1):57-64.
【9】WENG T I, CHEN M H, LIEN G W, et al. Effects of gender on the association of urinary phthalate metabolites with thyroid hormones in children:A prospective cohort study in Taiwan[J]. International Journal of Environmental Research and Public Health, 2017,14(2):123.
【10】朱效宁,汪国权,周志俊,等.尿中13种邻苯二甲酸酯代谢物的高效液相色谱串联质谱测定法[J].环境与职业医学, 2015,32(3):265-270.
【11】宋喜丽.固相萃取-超高效液相色谱-串联质谱法测定人尿中环境化学污染物代谢物[D].北京:中国疾病预防控制中心, 2017.
【12】HE X, ZANG J J, LIAO P, et al. Distribution and dietary predictors of urinary phthalate metabolites among pregnant women in Shanghai, China[J]. International Journal of Environmental Research and Public Health, 2019,16(8):1366.
【13】康莉,刘红河,廖仕成,等.电喷雾液相色谱串联质谱法测定人尿中10种邻苯二甲酸单酯[J].中国卫生检验杂志, 2017,27(23):3349-3351.
【14】张续,邱天,付慧,等.超高效液相色谱-三重四极杆质谱法测定人尿中9种邻苯二甲酸酯代谢物[J].色谱, 2018,36(9):895-903.
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