摘要
目的建立了超高效液相色谱-串联三重四级杆质谱(UPLC-MS/MS)测定母乳中游离态双酚A(BPA)的方法。方法 BPA经甲醇-丙酮(1∶1,V/V)超声提取后,过固相萃取柱(Waters Sep-Pak NH26 cc)进行净化,甲醇-丙酮(1∶1,V/V)洗脱,经Waters ACQUITY BEH C18色谱柱(50 mm×2.1mm×1.7μm)分离,在电喷雾负离子源和多反应监测模式下进行测定,内标法定量。结果 BPA在0.1～20μg/L范围内线性关系良好,相关系数r2>0.997。BPA的加标回收率为91.85%～106.75%,相对标准偏差为4.80%～15.36%,检出限为0.010μg/L,方法定量限为0.035μg/L。结论本方法可满足母乳中游离态双酚A含量评估的需要。
Objective A method was developed for determination of free bisphenol A （BPA） in human milk by ultra- performance liquid chromatography and tandem mass spectrometry （UPLC-MS/MS）. Methods BPA was ultrasonic extracted with methanol/acetone （1： 1, V/V）, purified by freezing-lipid coupled with solid phase extraction （Waters Sep- Pak NH2 6 cc）, and then eluted with methanol/acetone （1： 1, V/V）. Finally, BPA was separated on a Waters ACQUITYTM BEH C18 column （50 mm ×2.1 mm× 1.7 μm） and detected by negative electrospray ionization in multiple reactions monitoring mode. Results The linear range of BPA was 0.1 - 20 μg/L, and the correlation coefficient （ r^2 ） of the standard curve was above 0. 997. The mean recoveries for BPA with three spike levels were 91.85% - 106.75% , and the relative standard deviations were 4.80% - 15.36%. The limit of detection of the method was 0. 010 μg/L, and the limit of quantification was 0. 035 μg/L. Conclusion The method was proved to be suitable to evaluate the level of free BPA in human milk.
出处
《中国食品卫生杂志》
北大核心
2013年第1期24-28,共5页
Chinese Journal of Food Hygiene
基金
卫生行业科研专项"食品安全应急与监测预警技术研究和应用"(200902009)
