HPLC-MS/MS法同时测定育发化妆品中的13种违禁成分

Simultaneous determination of 13 prohibited drugs in hair growth cosmetics by HPLC-MS/MS

目的:建立可同时测定育发类化妆品中13种组分(米诺地尔、螺内酯、雌酮、坎利酮、黄体酮、非那雄胺、醋酸环丙孕酮、哈西奈德、氢化可的松、可的松、泼尼松、甲基泼尼松龙、地塞米松)含量的高效液相色谱串联三重四极杆质谱法(HPLC-MS/MS)。方法:采用菲罗门C18色谱柱(2.6μm,2.1 mm×100 mm),流动相为0.2%甲酸甲醇-0.2%甲酸水,梯度洗脱,流速为0.3 mL·min^-1,柱温为30℃。质谱条件:采用电喷雾离子源以正离子(ESI+)多反应监测模式(MRM)进行质谱监测。结果:在所设定的条件下,13种成分均分离良好,在考察的浓度范围内线性关系良好(r> 0.999);平均加标回收率:溶液型89.1%~100.3%;乳液型:88.3%~101.6%,RSD均<7.0%。结论:该方法高效、快捷、准确,可作为育发剂化妆品中非法添加违禁药物的快速检测方法。

Objective:To establish an HPLC-MS/MS method for the assay of 13 prohibited drugs in hair growth cosmetics,including minoxidil,prednisone,cortisone,hydrocortisone,dexamethasone,methylprednisolone,spironolactone,estrone,canrenone,finasteride1,cyproterone acetate,halcinonide,progesterone. Methods:The analytes were separated on a Phenomenex C18(2.6 μm,2.1 mm×100 mm)with the mobile phases of 0.2%(v/v)formic acid methanol and 0.2%(v/v)formic acid aqueous solution in gradient elution. The flow rate was 0.3 mL·min^-1,and the column temperature was 30 ℃. The electrospray ionization source with positive ion mode was used for analyzing the 13 prohibited drugs in the multiple reaction monitoring(MRM))mode. Results:Good separation for 13 compounds were obtained under the optimized chromatographic conditions,the calibration curves for 13 compounds were linear and the correlation coefficients were above 0.999 in the concentration range of the investigation. The recoveries of 13 compounds were 89.1%-100.3%(for liquid)and 88.3%-101.6%(for emulsion),and the relative standard deviations(RSDs)were bellow 7.0%. Conclusion:The method is accurate,sensitive and effective. It can be used for the quality control of hair growth cosmetics.