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目的建立测定饮用水中双酚A(BPA)和壬基酚(NP)的在线固相萃取-液质联用法(On-line SPE LC-MS/MS)。方法水样经On-line SPE在线富集和净化,以甲醇-水为在线固相萃取流动相,流速2.0ml/min,采用沃特世Direct Connect HP XBridgeTMC18在线固相萃取柱(填料粒径10μm)进行在线固相萃取。以甲醇-0.1%氨水为分析流动相,流速0.4ml/min,采用沃特世UPLC BEH C18色谱柱进行分析。质谱检测器采用电喷雾电离源,以多反应监测(MRM)方式进行负离子监测,采用内标法对饮用水中的BPA和NP进行定量分析。结果该方法每个样品总耗时10min。BPA线性范围为5～1000ng/L,NP为10～5000ng/L,相关系数(r2>0.999)。BPA、NP的定量限(LOQ)分别为5和10ng/L,两种内分泌干扰物在3个加标水平下平均回收率为86.6%～105%,相对标准偏差3.11%～18.2%,日间精密度11.3%～13.2%。结论该方法实现了样品的自动化前处理,提高了分析效率,操作简单,灵敏度高,可用于饮用水中两种环境内分泌干扰物的痕量检测。
Objective To establish an on-line SPE-LC / MS method for the determination of BPA and NP in drinking water. Methods Water samples were enriched and purified on-line by On-line SPE. The flow rate was 2.0ml / min with methanol-water as the mobile phase. Waters Direct Connect HP XBridgeTM C18 on-line solid phase extraction column ) For online solid-phase extraction. Methanol-0.1% aqueous ammonia was used as the mobile phase at a flow rate of 0.4 ml / min and analyzed on a Waters UPLC BEH C18 column. The mass spectrometry detector used the electrospray ionization source to carry out negative ion monitoring by multi-reaction monitoring (MRM). The internal standard method was used to quantitatively analyze BPA and NP in drinking water. As a result, the method took 10 minutes per sample. BPA linear range of 5 ~ 1000ng / L, NP 10 ~ 5000ng / L, correlation coefficient (r2> 0.999). The limits of quantitation (LOQ) of BPA and NP were 5 and 10 ng / L, respectively. The average recoveries of two endocrine disruptors at three spiked levels were 86.6% -105% and the relative standard deviations were 3.11% ~ 18.2% Precision 11.3% ~ 13.2%. Conclusion This method has realized the automated pre-treatment of samples, improved the analysis efficiency, simple operation, high sensitivity and can be used for the trace detection of two environmental endocrine disruptors in drinking water.