固相萃取-LC-MS/MS测定水中双酚A类物质

目的 建立固相萃取-液相色谱-串联质谱测定水中双酚类物质的高灵敏度方法。 方法 水样直接经反相C₁₈小柱浓缩净化。以乙腈-水为流动相进行梯度洗脱,采用液相色谱-质谱/质谱电喷雾负离子电离(ESI^-)模式和多反应监控(MRM)模式,以双酚A-d₁₆和四溴双酚A-d₁₀为内标进行定量。 结果 测定水中双酚F、双酚A、四氯双酚A和四溴双酚A的线性范围均为10~2 500 ng/L,线性相关系数分别为0.998、0.998、0.9998 和0.9990,检出限分别为5、2、0.2、2 ng/L,加标水平为250、1 000 ng/L时,双酚F、双酚A、四氯双酚A和四溴双酚A的回收率范围为65.3%～100.4%。 结论 固相萃取-液相色谱-串联质谱测定水中双酚类物质,方法简便,灵敏度高,选择性好,可作为检测水中四种双酚类物质的有效手段。

Determination of bisphenol A analogs in water sample by liquid chromatography-tandem mass spectrometry with solid phase extraction

Objective A high sensitivity method for determination of bisphenols in water by liquid chromatography-tandem mass spectrometry (LC-MS/MS) with solid phase extraction (SPE) was established. Methods The water samples were concentrated and purified by C18 cartridge directly, and then gradiently eluted with acetonitrile-water as the mobile phase for the baseline separation of the four compounds, bisphenol F (BPF), bisphenol A (BPA), tetrachlorobisphenol A (TCBPA ) and tetrabromobisphenol A (TBBPA), in thirteen minutes. BPA–d₁₆ and TBBPA–d₁₀ were used as internal standards and the analytes were identified by LC-MS/MS with the negative electrospray ionization under multiple reaction monitoring mode. Results The linear ranges of BPF, BPA, TCBPA and TBBPA in water all fell in 10ng/L-2,500ng/L. The linear correlation coefficients of their standard curves were 0.998, 0.998, 0.9998 and 0.9990 respectively, and the detection limits were 5ng/L, 2ng/L, 0.2ng/L and 2ng/L. The average recoveries for BPF, BPA, TCBPA and TBBPA at spiked concentration levels of 250 ng/L and 1000 ng/L were in the range of 65.3%~100.4%. Conclusions The LC-MS/MS coupled with SPE is simple, highly sensitive and selective. It provides an effective approch for the detection of bisphenols in water.