全自动固相萃取-超高效液相色谱-串联质谱法同时测定江水中8种酚类内分泌干扰物  

Simultaneous Determination of 8 Phenolic Endocrine Disrupting Chemicals in River Water by UHPLC-MS/MS with Automated Solid Phase Extraction

作　　者：华永有[1] 林麒[1] 卢翠英[1] HUA Yongyou;LIN Qi;LU Cuiying(Fujian Provincial Key Laboratory of Zoonosis Research,Fujian Center for Disease Control and Prevention,Fuzhou 350001,China)

机构地区：[1]福建省疾病预防控制中心福建省人兽共患病研究重点实验室

出　　处：《理化检验（化学分册）》2019年第8期904-911,共8页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：福建省自然科学基金（2015J01295）

摘　　要：移取江水样500mL,加入50.0μg·L^-1内标混合溶液100μL,采用全自动固相萃取仪(装有ENVI TM-18固相萃取柱)进行富集净化,收集洗脱液,于40℃水浴氮吹至近干,用乙腈(1+1)溶液定容至1.0mL,采用超高效液相色谱-串联质谱法同时测定其中8种酚类内分泌干扰物的含量。以HSS T3色谱柱为固定相,以不同体积比的0.1%(质量分数)氨水和乙腈的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾负离子源和多反应监测模式。采用内标法定量,8种酚类内分泌干扰物的线性范围均为0.10~40.00μg·L^-1,检出限(3S/N)为0.008~0.096ng·L^-1。方法用于闽江水样的分析,加标回收率为80.0%~91.8%,回收量的相对标准偏差(n=6)为2.9%~12%。The river water sample(500 mL)was collected and 50.0μg·L^-1 mixed solution of internal standard(100μL)were added.Enrichment and purification were processed by the instrument of automated solid phase extraction with ENVI TM-18 solid phase extraction column.The collected eluate was evaporated to near dryness by N2-blowing at 40℃in the water bath and then made up to 1.0 mL with acetonitrile(1+1)solution.UHPLCMS/MS was applied to the simultaneous determination of 8 phenolic endocrine disrupting chemicals in the solution.HSS T3 chromatographic column was used as stationary phase,and the mixture of 0.1%(mass fraction)ammonia and acetonitrile mixed in different ratios was used as mobile phase in gradient elution.ESI-and multi-reactions monitor mode were adopted in MS/MS.Internal standard method was used for quantitative.Linearity ranges of the 8 phenolic endocrine disrupting chemicals were found in the same range of 0.10-40.00μg·L^-1 with detection limits(3 S/N)in the range of 0.008-0.096 ng·L^-1.The proposed method was applied to the analysis of the water sample of Minjiang River,giving values of recovery found by standard addition method and RSDs(n=6)of recovery amounts in the ranges of 80.0%-91.8% and 2.9%-12% respectively.

关 键 词：超高效液相色谱-串联质谱法 酚类内分泌干扰物 江水 全自动固相萃取 

分 类 号：O657.63[理学—分析化学]