化妆品乳膏剂中双酚A测定的能力验证样品制备研究

Research on the sample preparation for proficiency testing of bisphenol A in cosmetic emulsion

目的研制用于能力验证(proficiency testing,PT)活动的化妆品乳膏剂中双酚A测定样品,建立供各参加实验室参考的化妆品乳膏剂中双酚A含量测定方法。方法采用乳化法制备O/W型双酚A乳膏剂,考察其理化指标、均匀性及稳定性。采用液相色谱-质谱法,以C18柱为固定相,甲醇和0.1%氨水(V/V)为流动相,梯度洗脱,电喷雾负离子模式(ESI-),多反应监测(MRM)扫描,对化妆品乳膏剂中双酚A进行定性定量分析。结果所制备样品理化指标、均匀性及稳定性符合相关要求。检测方法的线性范围为0.01μg/ml^1.0μg/ml,相关系数为0.999 8,检出限为0.005μg/ml,加标回收率为96.8%(RSD=2.3%)。结论样品理化指标良好、均匀、稳定,检测方法适用于乳膏剂中双酚A的定性定量分析,可用于后续开展的PT活动。

Objective To prepare a cosmetic emulsion sample for the proficiency testing（ PT） of bisphenol A（ BPA）,so as to establish an analytical method for the determination of BPA in cosmetic emulsion for participants＇ reference. Methods Using the emulsification method,O/W BPA emulsion was prepared. Its physical and chemical indexes,as well as homogeneity and stability,were analyzed. A method was developed for the determination of BPA contents in cosmetic emulsion using C18 column as separation column by high performance liquid chromatography-tandem mass spectrometry（ HPLC-MS/MS）,and gradient elution was performed with methanol-0. 1% ammonia（ V/V） as the mobile phase. The analyte was detected under multiple reaction monitoring（ MRM） with electrospray ionization in negative ion mode（ ESI-）. BPA in cosmetic emulsion was conducted for qualitative and quantitative analysis. Results The sample＇s physical and chemical indexes,homogeneity and stability could meet the requirements of performance testing. The linear ranges of the calibration curves for BPA was within 0. 01 μg/ml-1. 0 μg/ml,with the correlation coefficients（ r） of 0. 999 8; the limit of detection（ LOD） was 0. 005 μg/ml; the average recovery was 96. 8%,with relative standard deviation（ RSD） of 2. 3%. Conclusion The prepared testing samples has good physical and chemical indicators,homogeneity and stability,so the method is capable for the qualitative and quantitative analysis of BPA in cosmetic emulsion and the application of PT.