化妆品中克罗米通的测定与验证

Determination and Verification of Clomitone in Cosmetics

为建立化妆品中克罗米通的液相色谱检测方法和液质联用仪验证方法,将样品用甲醇超声提取10 min后,经滤膜过滤后液相色谱进样,采用C18色谱柱(4.6 mm×250 mm×5μm)分离,流动相为乙腈-质量分数1%三乙胺的磷酸二氢钾溶液(0.05 mol/L),用磷酸调体系pH至4.0(体积比40/60),二极管检测器分离,在波长242 nm下有最大吸收,标准曲线定量。结果发现,线性范围为10~500μg/mL,r>0.9999,检出限为20μg/g,空白膏霜、水剂及凝胶类化妆品在54.93、183.09及915.46μg等3个加标水平下的回收率为98.5%~109.5%,相对标准偏差为0.5%~3.1%。该方法操作简单,重现性好,适用于化妆品中克罗米通的测定。

To establish a method for the determination of Clomitone in cosmetics by liquid chromatography and a verification method for LC-MS,the sample was ultrasonically extracted with methanol for 10 min,filtered through a membrane and then injected into a liquid chromatography C18 column(4.6 mm×250 mm×5μm).The mobile phase was acetonitrile-1%(mass fraction)triethylamine potassium dihydrogen phosphate solution(0.05 mol/L),phosphoric acid was used to adjust pH of test system to 4.0(volume ratio 40/60),and the diode detector was used for separation.The wavelength of detection showed the maximun absorption at 242 nm,the standard curve was used for quantitative analysis.The results showed that the linear range was 10-500μg/mL,r>0.9999,the detection limit was 20μg/g,the recovery of blank cream,lotion and gel cosmetics spiked at three levels of 54.93,183.09 and 915.46μg were 98.5%-109.5%,and the relative standard deviation was 0.5%-3.1%.The method was simple to operate and has good reproducibility,which is suitable for the determination of Clomitone in cosmetics.