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目的基于少量样本,建立母乳中8种双酚类化合物(双酚A、双酚B、双酚E、双酚F、双酚S、双酚AF、双酚AP和双酚BP)快速灵敏的检测方法。方法母乳样品经乙腈超声萃取,冷冻去脂,丹磺酰氯衍生后采用超高效液相色谱串联质谱(UPLC-MS/MS)测定。采用ACQUITY UPLC BEH Phenyl柱(2.1 mm×100 mm,1.7μm)进行分离,以甲醇-0.1%甲酸水溶液为流动相,在电喷雾正离子源(ESI+)和多反应监测模式(MRM)下进行测定,同位素内标法定量,并对所建立的方法进行方法学考察。结果 8种化合物在0.010~10.00μg/L范围内线性关系良好(R2>0.99),3个水平的加标回收率为84.6%~108.1%,相对标准偏差<12%(n=6)。利用该方法分析了30份母乳样品,11份母乳样品有双酚A检出,浓度范围为0.13~2.25μg/L;1份样品检测到双酚AF,浓度为0.02μg/L。结论该方法母乳用量少,灵敏度高,简便快捷,可用于母乳中8种双酚类物质的同时测定。
OBJECTIVE To establish a fast and sensitive method for the determination of 8 bisphenols (BPA, BPA, BPA, BPA, BPA, BPA, BPA and BPBP) in breast milk based on a few samples Detection method. Methods Breast milk samples were extracted with acetonitrile, frozen and degreased, and dansyl chloride derivatized by UPLC-MS / MS. The separation was carried out on an ACQUITY UPLC BEH Phenyl column (2.1 mm × 100 mm, 1.7 μm) and the reaction was carried out using a mobile phase of methanol-0.1% formic acid in electrospray positive ionization (ESI +) and multiple reaction monitoring (MRM) , The internal standard method of isotope quantification, and methodological study of the established method. Results The linearity of the eight compounds in the range of 0.010-10.00 μg / L was good (R2> 0.99). The recoveries of the three compounds were 84.6% -108.1% and the relative standard deviations were less than 12% (n = 6). Using this method, 30 samples of breast milk were analyzed, and 11 samples of milk samples were detected with bisphenol A in the concentration range of 0.13 ~ 2.25μg / L. Bisphenol AF was detected in one sample with a concentration of 0.02μg / L. Conclusion The method of breast milk with less, high sensitivity, simple and quick, can be used for the determination of eight bisphenols in breast milk at the same time.