Wang Ping, Ding Xiaojing, Li Yun, Yang Yuanyuan
Beijing Center for Disease Control and Prevention, Beijing 100013, People's Republic of China.
J AOAC Int. 2012 Jul-Aug;95(4):1069-73. doi: 10.5740/jaoacint.11-043.
A new method for the simultaneous quantitation of 11 preservatives-imidazolidinyl urea, benzyl alcohol, dehydroacetic acid, sorbic acid, phenoxyethanol, benzoic acid, salicylic acid, and four parabens (methyl, ethyl, propyl, and butyl)-in cosmetics by micellar electrokinetic capillary chromatography was established and validated. The separation was performed using an uncoated fused-silica capillary (50 pm id x 60.2 cm, effective length 50 cm) with a running buffer consisting of 15 mmol/L sodium tetraborate, 60 mmol/L boric acid, and 100 mmol/L sodium dodecyl sulfate. A 1:10 dilution of the running buffer was used as the sample buffer to extract the cosmetic samples. The key factors, such as the concentration and pH of the running and sample buffers, which influence quantitative analysis of the above 11 preservatives in cosmetic samples, were investigated in detail. The linear ranges of the calibration curves for imidazolidinyl urea and the other 10 preservatives were 50-1000 and 10-200 mg/L, respectively. The correlation coefficients of the standard curves were all higher than 0.999. The recoveries at the concentrations studied ranged from 93.0 to 102.7%. RSDs were all less than 5%. The new method with simple sample pretreatment met the needs for routine analysis of the 11 preservatives in cosmetics.
建立并验证了一种通过胶束电动毛细管色谱法同时定量化妆品中11种防腐剂(咪唑烷基脲、苯甲醇、脱氢乙酸、山梨酸、苯氧乙醇、苯甲酸、水杨酸以及四种对羟基苯甲酸酯类——甲酯、乙酯、丙酯和丁酯)的新方法。分离使用未涂层熔融石英毛细管(内径50μm×60.2cm,有效长度50cm),运行缓冲液由15mmol/L四硼酸钠、60mmol/L硼酸和100mmol/L十二烷基硫酸钠组成。运行缓冲液1:10的稀释液用作样品缓冲液来提取化妆品样品。详细研究了运行缓冲液和样品缓冲液的浓度及pH等影响化妆品样品中上述11种防腐剂定量分析的关键因素。咪唑烷基脲和其他10种防腐剂校准曲线的线性范围分别为50 - 1000mg/L和10 - 200mg/L。标准曲线的相关系数均高于0.999。在所研究浓度下的回收率为93.0%至102.7%。相对标准偏差均小于5%。这种样品前处理简单的新方法满足了化妆品中11种防腐剂常规分析的需求。