脐带血清中五种邻苯二甲酸酯代谢产物的固相萃取高效液相色谱-质谱测定法  

Determination of five phthalate metabolites in cord serum by solid phase extraction high performance liquid chromatography-mass spectrometry

作　　者：杨叶[1] 蔡岩[1] 燕美玲[1] 陈曦[1] 高娜[1] 姬亚芹[2] 孙增荣[1] 

机构地区：[1]天津医科大学公共卫生学院,天津300070 [2]南开大学环境科学与工程学院

出　　处：《环境与健康杂志》2012年第11期1039-1042,共4页Journal of Environment and Health

基　　金：天津市科技支撑计划重点项目(09ZCGYSF01700)

摘　　要：目的建立脐带血清中的邻苯二甲酸酯(PAEs)代谢产物的高效液相色谱-质谱测定方法。方法采用β-葡萄糖酸酐酶水解脐带血清中结合型邻苯二甲酸酯代谢物,酶解后的溶液采用固相萃取法富集净化,采用高效液相色谱-串联质谱法对脐带血清中5种邻苯二甲酸单酯代谢产物[邻苯二甲酸单甲酯(MMP)、邻苯二甲酸单乙酯(MEP)、邻苯二甲酸单丁酯(MBP)、邻苯二甲酸单丁苄酯(MBzP)、邻苯二甲酸-单-乙基己基酯(MEHP)]进行测定,流动相为乙腈(0.1%乙酸)与水(0.1%乙酸)梯度洗脱,流量为0.3 ml/min。结果在0.3～800μg/L的线性范围内,5种待测邻苯二甲酸单酯MMP、MEP、MBP、MBzP、MEHP的回归方程均呈良好的线性关系,相关系数均>0.99,检出限为0.109～0.579μg/L,平均回收率在80.59%～85.75%之间,RSD在3.09%～3.91%之间。结论该方法回收率较高,重现性较好,适用于脐带血清中5种邻苯二甲酸单酯的同时测定。Objective To establish a method for the determination of phthalate metabolites in cord serum by high performance liquid chromatography-mass spectrometry. Methods After treated with β-glucuronidase, the cord serum samples were subjected to the solid phase extraction column to clean-up and concentrate. The contents of the five kinds of phthalates metabolites （MMP, MEP, MBP, MBzP and MEHP） were determined by using high performance liquid chromatography-mass spectrometer, a mixture of methyl cyanides（0.1% acetic acid） and water（0.1% acetic acid） was used as mobile phase to gradient elution, the flow rate was 0.3 ml/min. Results The linear range was 0.3-800 μg/L for the five kinds of phthalates metabolites （MMP, MEP, MBP, MBZP and MEHP） with good correlation coefficient （R2〉0.99）. The limits of detection ranged from 0.109 μg/L to 0.579 μg/L, the average recovery rates were 80.59%-85.75%, and the relative standard deviation were 3.09%- 3.91%. The detectable rates of MMP, MEP, MBP, MBzP and MEHP in 30 cord serum samples were 100.0%, 93.3%, 83.3%, 93.3%, 100.0%, and the medians were 16.01 μg/L, 4.37 μg/L, 9.67 μg/L, 1.58 μg/L, 5.31 μg/L, respectively. Conclusion This method has good recovery rate and reproducibility, is suitable for the determination of five kinds of phthalate metabolites in cord serum.

关 键 词：色谱法 液相 邻苯二甲酸酯 脐带 血清 固相萃取 质谱 

分 类 号：O657.7[理学—分析化学]