Schettino Lorenza, Benedé Juan L, Chisvert Alberto
GICAPC Research Group, Department of Analytical Chemistry, University of Valencia 46100 Burjassot Valencia Spain
RSC Adv. 2023 Jan 19;13(5):2963-2971. doi: 10.1039/d2ra06553c. eCollection 2023 Jan 18.
An analytical method for the simultaneous determination of nine prohibited -nitrosamines in cosmetic products is presented. -nitrosamines are banned compounds in cosmetic products due to their harmful effects. Therefore, these compounds are not intentionally added to these products but, however, small amounts of them may be present due to unintentional causes, and thus sensitive methods for their analytical control are required. The proposed method is based on vortex-assisted dispersive liquid-liquid microextraction (VA-DLLME) to extract and preconcentrate the analytes, followed by gas chromatography-mass spectrometry (GC-MS) for their determination. The variables involved in the VA-DLLME process were optimized by using a Box-Behnken design and, due to the different polarity of the -nitrosamines studied, several approaches for sample treatment were compared to achieve the best results. The method was successfully validated, showing a good linearity at least up to 20 ng mL, enrichment factors from 2 to 100 depending on the target analyte, limits of detection and quantification at the low μg kg level, and good repeatability values (<13%). Finally, the proposed analytical method was applied to the determination of -nitrosamines in commercial cosmetic samples of different nature, avoiding the matrix effect by means of standard addition calibration. Significant amounts of some of the -nitrosamines, even exceeding the established regulatory limit, were found in the samples. The resulting method is fast, simple, and affordable to carry out the quality control of cosmetic products to ensure consumer safety for most laboratories.
本文提出了一种同时测定化妆品中九种禁用亚硝胺的分析方法。由于亚硝胺具有有害影响，它们在化妆品中属于禁用化合物。因此，这些化合物并非有意添加到这些产品中，然而，由于意外原因可能会存在少量亚硝胺，所以需要灵敏的分析控制方法。所提出的方法基于涡旋辅助分散液液微萃取（VA-DLLME）来萃取和预富集分析物，随后采用气相色谱-质谱联用（GC-MS）进行测定。通过使用Box-Behnken设计对VA-DLLME过程中涉及的变量进行了优化，并且由于所研究的亚硝胺极性不同，比较了几种样品处理方法以获得最佳结果。该方法成功得到验证，至少在20 ng/mL范围内显示出良好的线性，富集因子根据目标分析物在2至100之间，检测限和定量限在低μg/kg水平，并且具有良好的重复性值（<13%）。最后，所提出的分析方法应用于不同性质的商业化妆品样品中亚硝胺的测定，通过标准加入校准避免了基质效应。在样品中发现了一些亚硝胺的大量存在，甚至超过了既定的监管限值。所得到的方法快速、简单且成本低廉，可用于化妆品的质量控制，以确保大多数实验室的消费者安全。
