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    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

    • 摘要: 移取江水样500 mL,加入50.0 μg·L-1内标混合溶液100 μL,采用全自动固相萃取仪(装有ENVITM-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1.0 mL,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0.10~40.00 μg·L-1,检出限(3S/N)为0.008~0.096 ng·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%。

       

      Abstract: The river water sample (500 mL) was collected and 50.0 μg·L-1 mixed solution of internal standard (100 μL) were added. Enrichment and purification were processed by the instrument of automated solid phase extraction with ENVITM-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. UHPLC-MS/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 0.10-40.00 μg·L-1 with detection limits (3S/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.

       

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