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目的建立尿液中5种邻苯二甲酸酯代谢产物的固相萃取-高分辨质谱测定法。方法尿样经β-葡萄糖苷酸酶水解后,以甲酸+水和甲酸+乙腈为流动相进行梯度洗脱,采用Oasis MAX固相萃取柱净化,Hypersil GOLD C18柱分离,再使用超高压液相色谱-高分辨率质谱仪进行定性和定量分析。结果在1~500μg/L的线性范围内,5种邻苯二甲酸酯代谢产物的回归方程的线性关系良好,r≥0.999 6。该方法对5种邻苯二甲酸酯代谢产物的检出限分别为0.03~0.39μg/L,定量下限分别为0.10~1.17μg/L;平均回收率为71.1%~104.3%,RSD为3.78%~9.64%。结论该方法的准确度和精密度均较好,回收率高,检出限较低,可用于人体尿液中5种邻苯二甲酸酯代谢产物的同时检测。
Objective To establish a method for the determination of 5 phthalate metabolites in urine by high performance liquid chromatography-high resolution mass spectrometry. Methods Urine samples were hydrolyzed by β-glucuronidase and eluted with formic acid + water and formic acid + acetonitrile as mobile phases. The samples were purified by Oasis MAX solid phase extraction column and separated on a Hypersil GOLD C18 column. Chromatography - High-resolution mass spectrometry for qualitative and quantitative analysis. Results In the linear range of 1 ~ 500μg / L, the regression equation of five phthalate metabolites showed a good linear relationship, r≥0.9996. The detection limits of the five phthalates metabolites were 0.03 ~ 0.39μg / L, the limits of quantification were 0.10 ~ 1.17μg / L, the average recovery was 71.1% ~ 104.3%, the RSD was 3.78 % ~ 9.64%. Conclusion The method has good accuracy and precision, high recovery and low detection limit. It can be used for the simultaneous detection of five phthalate metabolites in human urine.