摘要
目的建立的测定孕妇血清中游离型双酚A的浓度同相萃取-同位素内标-高效液相色谱串联质谱（HPLC—MS／MS）法。方法采用OasisHLB同相萃取柱进行固相萃取，液相色谱的分离采用C18色谱柱，使用乙腈和水作为流动相进行梯度洗脱。质谱运用负离子喷雾模式电离，多反应离子监测方式检测。结果该方法检测双酚A的线性范围为0．2-50ng／ml，r=0．9999，最低检测限为0．15ng／ml，定量限为0．4ng／ml。0．5、2、10、50ng/ml 4个浓度的加标回收率分别为114．8％，108．1％，100．8％，97.2％；日内RSD分别为15．9％，9.3％，4．6％，3．5％；日问RSD分别为10．5％，15．1％，53％，5．1％。结论该方法测定孕妇血清中游离型双酚A具有较高的灵敏度、特异度和精确性，适用于血清样本中痕量双酚A的检测。
Objective To estabhsh a method using isotope dilution-solid phase extraction （SPE） coupled to high-pefformnce liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） for the determination of free bisphenol A （BPA） concentration in human serum sample. Methods The Oasis HLB SPE column was used for the concentration and extraction of BPA in the serum. C18ehromatographie column was used with a gradient elution system of acetonitrile-water as the mobile phase, mass spectrometry under negative electrospray ionization mode and nmhiple reaction monitoring （MRM） were performed for the qualitative and quantitative analysis. Results The linear range was 0.2-50 ng/ml, r =0.999 9. The limit of detection and quantification were 0.15 ng/ml and 0.4 ng/ml respectively. The spiked recoveries of BPA in serum samples of 0.5, 2, 10 and 50 ng/ml were 114.8%, 108.1%, 100.8% and 97.2%, respectively. Conclusion The method using isotope dilution-solid phase extraction （SPE） coupled to high-pcffomlanee liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） for the determination of free bisphenol A （BPA） eoncentration in human serum sample has high sensitivity, selectivity and precision, and is applicable to the measurement of trace level BPA in the serum.
出处
《环境与健康杂志》
CAS
CSCD
北大核心
2014年第1期44-46,共3页
Journal of Environment and Health
基金
国家自然科学基金(81072310)
安徽省学术和技术带头人及后备人选科研资助项目(2012-5)
安徽医科大学博士科研资助项目(XJ201019
XJ201204)
关键词
双酚A
血清
固相萃取
高效液相色谱-串联质谱
Bisphenol A
Serum
Solid phase extraction （SPE）
High-performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）
