De Orsi Daniela, Pellegrini Manuela, Pichini Simona, Mattioli Donatella, Marchei Emilia, Gagliardi Luigi
Department of Therapeutic Research and Medicines Evaluation, Istituto Superiore di Sanità, V.le Regina Elena 299, 00161 Rome, Italy.
J Pharm Biomed Anal. 2008 Nov 4;48(3):641-8. doi: 10.1016/j.jpba.2008.06.008. Epub 2008 Jun 25.
A simple high-performance liquid chromatography (HPLC) method with ultraviolet diode array (UV-DAD) and electrospray ionisation mass spectrometry (ESI-MS) detection has been developed for the determination of minoxidil, progesterone, estrone, spironolactone, canrenone, hydrocortisone and triamcinolone acetonide in cosmetic products. The presence of these substances in commercial cosmetic samples is prohibited. The compounds were separated by reversed phase chromatography with water (0.1% trifluoroacetic acid) and acetonitrile gradient elution and detected by UV-DAD at 230, 254 and 280 nm and by ESI-MS positive ionisation mode. Benzoic acid was used as internal standard. Linearity was studied with UV-DAD detection from 1.50 to 1,000 microg/ml or mug/g range, depending on the different compounds and type of cosmetic preparation and with ESI-MS in the 50-1,000 ng/ml or ng/g range. Good determination coefficients (r(2)>or=0.99) were found in both UV and ESI-MS. At three concentrations spanning the linear dynamic ranges of both UV-DAD and ESI-MS assay, mean recoveries were always higher than 90% for the different analytes. This method was successfully applied to the analysis of substances under investigations illegally added in cosmetic cream and lotions, sold on internet web sites to prevent hair loss and other hormone-dependent skin diseases, like acne and hirsutism.
已开发出一种采用紫外二极管阵列（UV-DAD）和电喷雾电离质谱（ESI-MS）检测的简单高效液相色谱（HPLC）方法，用于测定化妆品中的米诺地尔、孕酮、雌酮、螺内酯、坎利酮、氢化可的松和曲安奈德。商业化妆品样品中禁止含有这些物质。化合物通过反相色谱法分离，以水（0.1%三氟乙酸）和乙腈梯度洗脱，并通过UV-DAD在230、254和280 nm处检测，以及通过ESI-MS正离子化模式检测。苯甲酸用作内标。根据不同化合物和化妆品制剂类型，采用UV-DAD检测在1.50至1000μg/ml或μg/g范围内研究线性，采用ESI-MS在50至1000 ng/ml或ng/g范围内研究线性。在UV和ESI-MS中均发现良好的测定系数（r²≥0.99）。在跨越UV-DAD和ESI-MS测定线性动态范围的三个浓度下，不同分析物的平均回收率始终高于90%。该方法成功应用于分析在互联网网站上销售的用于防止脱发和其他激素依赖性皮肤病（如痤疮和多毛症）的面霜和乳液中非法添加的调查物质。
