摘要
为扩大检验范围,优化化妆品检验能力,本研究建立了高效液相色谱法同时测定化妆品中己脒定二盐等7种防腐剂的含量。对不同基质类型的化妆品样品加入提取溶剂超声提取,提取液经高速离心处理,上清液以正己烷脱脂,经0.45微孔滤膜过滤后取续滤液测定。色谱柱为C18(4.6 mm×250 mm,5μm),以0.1%三氟乙酸水溶液和乙腈为流动相梯度洗脱,检测器为二极管阵列检测器(DAD),采用外标法定量。在该条件下,7种防腐剂均在其线性范围内,线性相关系数≥0.997。三种不同剂型空白基质在低、中、高3个质量浓度加标水平下,方法的平均回收率为99.6%~111.1%,相对标准偏差(n=6)≤2.9%。该测定方法具有特异性显著,灵敏度、准确度高,适用于化妆品中该类防腐剂的检测。
To expand detection range and modify the needs of inspection in cosmetics,the determination of hexamidine and other 6 kinds of preservatives was established by performance liquid chromatography.Different forms of cosmetic samples were treated by ultrasonic extration,the extration solution was obtained by high-speed centrifugation,the supernatant was degreased by hexane and then filtered by 0.45μm millipore filter.Chromatographic operation was conducted on C18 column(4.6 mm×250 mm,5μm)by a gradient elution of 0.1%aqueous trifluoroacetic acid solution and acetonitrile.The detection was completed using a diode array detector(DAD).The external standard method was used for quantitation.Under the optimum conditions,good linearity was observed over a certain range of concentration,the results showed that their linear ranges were above 0.997,the mean recoveries were 99.6%to 111.1%,relative standard deviation was below 2.9%(n=6)at three mass concentration gradients of low,medium and high for three different types of matrixes.The method was proved to be high specified,sensitive and accurate,it could be used in the practical determination of commercial cosmetics.
作者
程红新
王福鑫
CHENG Hongxin;WANG Fuxin(Liaoning Institute for Drug Control,Shenyang 110036,China)
