尿液中5種鄰苯二甲酸酯代謝產(chǎn)物的高效液相色譜-串聯(lián)質(zhì)譜測定法
發(fā)布時間:2018-01-07 10:07
本文關鍵詞:尿液中5種鄰苯二甲酸酯代謝產(chǎn)物的高效液相色譜-串聯(lián)質(zhì)譜測定法 出處:《環(huán)境與健康雜志》2017年07期 論文類型:期刊論文
更多相關文章: 鄰苯二甲酸酯代謝產(chǎn)物 固相萃取 超高壓液相色譜-高分辨率質(zhì)譜 尿
【摘要】:目的建立尿液中5種鄰苯二甲酸酯代謝產(chǎn)物的固相萃取-高分辨質(zhì)譜測定法。方法尿樣經(jīng)β-葡萄糖苷酸酶水解后,以甲酸+水和甲酸+乙腈為流動相進行梯度洗脫,采用Oasis MAX固相萃取柱凈化,Hypersil GOLD C18柱分離,再使用超高壓液相色譜-高分辨率質(zhì)譜儀進行定性和定量分析。結(jié)果在1~500μg/L的線性范圍內(nèi),5種鄰苯二甲酸酯代謝產(chǎn)物的回歸方程的線性關系良好,r≥0.999 6。該方法對5種鄰苯二甲酸酯代謝產(chǎn)物的檢出限分別為0.03~0.39μg/L,定量下限分別為0.10~1.17μg/L;平均回收率為71.1%~104.3%,RSD為3.78%~9.64%。結(jié)論該方法的準確度和精密度均較好,回收率高,檢出限較低,可用于人體尿液中5種鄰苯二甲酸酯代謝產(chǎn)物的同時檢測。
[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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