HPLC-HRMS法测定小鼠组织中的邻苯二甲酸酯  

Determination of Phthalate Esters in Mouse Tissues by HPLC-HRMS

作　　者：毛淑娟 竺美 唐文雅 林鑫 吴淼 杨秋燕 邓伟 MAO Shu-juan;ZHU Mei;TANG Wen-ya;LIN Xin;WU Miao;YANG Qiu-yan;DENG Wei(Sichuan Academy of Environmental Sciences,Chengdu 610041,China)

机构地区：[1]四川省生态环境科学研究院,成都610041

出　　处：《四川环境》2025年第2期126-133,共8页Sichuan Environment

基　　金：四川省生态环境科学研究院自有基金科技创新项目(2022-079)。

摘　　要：建立了超声提取-液相色谱串联高分辨质谱法测定小鼠羊水、胚胎、胎盘样品中邻苯二甲酸酯类化合物(phthalate esters,缩写PAEs)的含量。通过开展针对生物组织痕量PAEs的多种前处理技术的应用实验,得到最佳条件为:称取0.1g样品经过5mL乙腈超声提取,离心后上清液经玻璃中性氧化铝小柱净化,液相色谱串联高分辨质谱仪全扫描模式内标法定量分析。结果表明,6种PAEs在质量浓度为2~50μg/L范围内线性良好,相关系数R在0.9994~0.9999,检出限在2.8~4.2μg/kg之间,样品加标平均回收率为88.2%~105%,RSD为9.0%~15%。该方法样品前处理简单,测试结果重复性和准确度较高,适用于低样品量、低含量小鼠组织中PAEs的测定。We established an ultrasound extraction-liquid chromatography-high resolution mass spectrometry/mass spectrometry to determine the content of phthalate esters(PAEs)in amniotic fluid,embryo,and placental samples of mouse.Through application experiments on various pre-treatment technologies for trace amounts of PAEs in biological tissues,the optimal conditions were determined as follows:Weighed 0.1 g samples and extracted them with 5 mL acetonitrile,and proceed with supersonic extraction;after centrifugation,purify the supernatant with a glass neutral alumina column,and quantitatively analyze the supernatant by liquid chromatography-high resolution mass spectrometry/mass spectrometry in full scan mode with the internal standard method.The results showed that the six PAEs exhibited good linearity within the mass concentration range of 2~50μg/L,the correlation coefficient R was in the range of 0.9994 to 0.9999,and the detection limit was in the range of 2.7~4.2μg/kg,the average recovery rate of the spiked samples was 88.2%~105%,and RSD was 9.0%~15%.With the method,sample pretreatmentis simple,and test results are of high repeatability and accuracy.To sum up,the method is suitable for determination of PAEs in mouse tissues of low sample size and low content.

关 键 词：超声提取 HPLC-HRMS 邻苯二甲酸酯 小鼠 

分 类 号：X174[环境科学与工程—环境科学]