尿液中5种邻苯二甲酸酯代谢产物的高效液相色谱-串联质谱测定法
发布时间:2018-01-07 10:07
本文关键词:尿液中5种邻苯二甲酸酯代谢产物的高效液相色谱-串联质谱测定法 出处:《环境与健康杂志》2017年07期 论文类型:期刊论文
更多相关文章: 邻苯二甲酸酯代谢产物 固相萃取 超高压液相色谱-高分辨率质谱 尿
【摘要】: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。
[Abstract]:Objective to establish a solid phase extraction (SPE)-high resolution mass spectrometry (HRMS) method for the determination of five metabolites of phthalates in urine. Methods urine samples were hydrolyzed by 尾-glucuronidase. The gradient elution was carried out with formic acid water and formic acid acetonitrile as mobile phase. The separation was performed on a Hypersil GOLD C18 column with Oasis MAX solid-phase extraction column. The qualitative and quantitative analysis were carried out by using the ultra-high pressure liquid chromatography-high resolution mass spectrometer. The results were linear in the range of 1 渭 g / L. The regression equation of five phthalate metabolites has a good linear relationship. R 鈮,
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