Giaccone Vita, Polizzotto Giuseppe, Macaluso Andrea, Cammilleri Gaetano, Ferrantelli Vincenzo
Istituto Zooprofilattico Sperimentale della Sicilia "A. Mirri", Via Gino Marinuzzi 3, 90129 Palermo, Italy.
Int J Anal Chem. 2017;2017:3531649. doi: 10.1155/2017/3531649. Epub 2017 Feb 14.
The aim of our present work was the development of a rapid high-performance liquid chromatography method with electrospray ionization and tandem mass spectrometry detection (LC-ESI-MS/MS) for the determination of several corticosteroids in cosmetic products. Corticosteroids are suspected to be illegally added in cosmetic preparations in order to enhance the curative effect against some skin diseases. Sample preparation step consists in a single extraction with acetonitrile followed by centrifugation and filtration. The compounds were separated by reversed-phase chromatography with water and acetonitrile (both with 0.1% formic acid) gradient elution and detected by ESI-MS positive and negative ionization mode. The method was validated at the validation level of 0.1 mg kg. Linearity was studied in the 5-250 g L range and linear coefficients () were all over 0.99. The accuracy and precision of the method were satisfactory. The LOD ranged from 0.085 to 0.109 mg kg and the LOQ from 0.102 to 0.121 mg kg. Mean recoveries for all the analytes were within the range 91.9-99.2%. The developed method is sensitive and useful for detection, quantification, and confirmation of these corticosteroids in cosmetic preparations and can be applied in the analysis of the suspected samples under investigation.
我们当前工作的目的是开发一种快速高效液相色谱法，结合电喷雾电离和串联质谱检测（LC-ESI-MS/MS）来测定化妆品中的几种皮质类固醇。怀疑皮质类固醇被非法添加到化妆品制剂中以增强对某些皮肤病的治疗效果。样品制备步骤包括用乙腈进行单次萃取，然后离心和过滤。化合物通过反相色谱法，以水和乙腈（均含有0.1%甲酸）梯度洗脱进行分离，并通过ESI-MS正离子和负离子电离模式进行检测。该方法在0.1 mg kg的验证水平下进行了验证。在5 - 250 g L范围内研究了线性关系，线性系数（）均超过0.99。该方法的准确度和精密度令人满意。检测限范围为0.085至0.109 mg kg，定量限范围为0.102至0.121 mg kg。所有分析物的平均回收率在91.9 - 99.2%范围内。所开发的方法对于化妆品制剂中这些皮质类固醇的检测、定量和确证是灵敏且有用的，可应用于对受调查的可疑样品的分析。
