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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 metabolites of phthalates (PAEs) in umbilical cord blood by high performance liquid chromatography-mass spectrometry. Methods β-Glucosidase was used to hydrolyze the bound phthalate metabolites in umbilical cord serum. The enzymatic solution was purified by solid-phase extraction and purified by high performance liquid chromatography-tandem mass spectrometry Phthalate monoester metabolites [monomethyl phthalate (MMP), monoethyl phthalate (MEP), monobutyl phthalate (MBP), monobutyl phthalate (MBzP), mono-ethylhexyl phthalate (MEHP)]. The mobile phase consisted of a gradient of acetonitrile (0.1% acetic acid) and water (0.1% acetic acid) with a flow rate of 0.3 ml / min. Results The linear regression equations of the five phthalates measured, MMP, MEP, MBP, MBzP and MEHP in the linear range of 0.3 ~ 800μg / L showed a good linear relationship with correlation coefficients> 0.99. The detection limits 0.109 ~ 0.579μg / L, the average recoveries ranged from 80.59% to 85.75%, RSD ranged from 3.09% to 3.91%. Conclusion The method has high recovery rate and good reproducibility, and is suitable for the simultaneous determination of five phthalate monoesters in cord serum.