Wang Bin, Niu Yumin, Zhang Jing, Shao Bing, Zhang Min
Tianjin University of Science & Technology, College of Food Engineering and Biotechnology, Tianjin 300457, China.
Wei Sheng Yan Jiu. 2017 Nov;46(6):965-970.
To establish a rapid and sensitive method for the analysis of eight bisphenols in breast milk using small amount of samples.
Breast milk samples were extracted by acetonitrile and the lipid substances were removed by freezing under-20 ℃ condition. Then the samples were derivatized with dansyl chloride and analyzed by ultra-performance liquid chromatography-tandem mass spectrometry( UPLCMS/MS). The seperation was performed on an ACQUITY UPLC BEH Phenyl column( 2. 1 mm × 100 mm, 1. 7 μm) with methanol and 0. 1% formic acid in water as mobile phase. The electrospray source was in the positive ion mode and monitored in the multiple reactions monitoring mode. Isotope internal standard dilution technique was used for the quantification analysis. At last, the methodology was studied.
The linear range of 8 bisphenols was 0. 010-10. 00 μg/L. The recoveries of the three spiked levels were84. 6%-108. 1%, with the relative standard deviations no more than 12%( n = 6). 30 samples of breast milk were analyzed, in which BPA was detected in 11 breast milk samples, and the concentrations ranged from 0. 13 μg/L to 2. 25 μg/L. BPAF was detected in 1 breast milk sample, and the concentration was 0. 02 μg/L.
The established method using a small amount of breast milk is highly sensitive, simple and fast, and can be used for the simultaneous determination of 8 bisphenols in breast milk.
建立一种使用少量样品分析母乳中8种双酚的快速灵敏方法。
母乳样品用乙腈萃取，在-20℃条件下冷冻去除脂质物质。然后样品用丹磺酰氯衍生化，采用超高效液相色谱-串联质谱法（UPLC-MS/MS）分析。分离在ACQUITY UPLC BEH苯基柱（2.1mm×100mm，1.7μm）上进行，以甲醇和0.1%甲酸水溶液为流动相。电喷雾源处于正离子模式，在多反应监测模式下进行监测。采用同位素内标稀释技术进行定量分析。最后，对该方法进行了研究。
8种双酚的线性范围为0.010-10.00μg/L。三个加标水平的回收率为84.6%-108.1%，相对标准偏差不超过12%（n=6）。分析了30份母乳样品，其中11份母乳样品中检测到双酚A，浓度范围为0.13μg/L至2.25μg/L。在1份母乳样品中检测到双酚AF，浓度为0.02μg/L。
所建立的使用少量母乳的方法灵敏度高、简单快速，可用于同时测定母乳中的8种双酚。
