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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、2ng/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。
OBJECTIVE To establish a high sensitivity method for the determination of bisphenols in water by solid phase extraction-liquid chromatography-tandem mass spectrometry. Methods The water samples were concentrated and purified directly by reverse phase C18 cartridge. The mobile phase was eluted with acetonitrile-water as mobile phase. The mobile phase was eluted with liquid chromatography-mass spectrometry / mass spectrometry electrospray ionization (ESI-) mode and multiple reaction monitoring (MRM) -d10 for internal standard quantification. Results The linear range of bisphenol F, bisphenol A, tetrachloro bisphenol A and tetrabromobisphenol A were 10-2 500 ng / L, and the linear correlation coefficients were 0.998, 0.998, 0.9999 and 0.9990, respectively. The recoveries of bisphenol F, bisphenol A, tetrachlorobisphenol A and tetrabromobisphenol A ranged from 5, 2, 0.2, 2 ng / L and spiked levels of 250 to 1 000 ng / L, respectively 65.3% ~ 100.4%. Conclusion Solid phase extraction - liquid chromatography - tandem mass spectrometry (HPLC-MS / MS) is a simple, sensitive and selective method for determination of bisphenols in water. It can be used as an effective method to detect four bisphenols in water.