摘要
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—d10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10～2500ng／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、1000ng／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 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 stand- ard 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.
出处
《实用预防医学》
CAS
2016年第10期1260-1263,共4页
Practical Preventive Medicine
关键词
液相色谱
质谱
固相萃取
双酚A
Liquid Chromatography
Mass Spectrometry
Solid phase extraction
Bisphenol A
