Comprehensive identification and quantitation of 100 multi-class regulated ingredients in cosmetics was achieved using ultra-high-performance liquid chromatography (UHPLC) coupled with hybrid quadrupole-Orbitrap high-resolution mass spectrometry (Q-Orbitrap HRMS). A simple, efficient, and inexpensive sample pretreatment protocol was developed using ultrasound-assisted extraction (UAE), followed by dispersive solid-phase extraction (dSPE). The cosmetic samples were analyzed by UHPLC-Q-Orbitrap HRMS under synchronous full-scan MS and data-dependent MS/MS (full-scan MS¹/dd-MS²) acquisition mode. The mass resolution was set to 70,000 FWHM (full width at half maximum) for full-scan MS¹ and 17,500 FWHM for dd-MS² stage with the experimentally measured mass deviations of less than 2 ppm (parts per million) for quasi-molecular ions and 5 ppm for characteristic fragment ions for each individual analyte. An accurate-mass database and a mass spectral library were built in house for searching the 100 target compounds. Broad screening was conducted by comparing the experimentally measured exact mass of precursor and fragment ions, retention time, isotopic pattern, and ionic ratio with the accurate-mass database and by matching the acquired MS/MS spectra against the mass spectral library. The developed methodology was evaluated and validated in terms of limits of detection (LODs), limits of quantitation (LOQs), linearity, stability, accuracy, and matrix effect. The UHPLC-Q-Orbitrap HRMS approach was applied for the analysis of 100 target illicit ingredients in 123 genuine cosmetic samples, and exhibited great potential for high-throughput, sensitive, and reliable screening of multi-class illicit compounds in cosmetics.

使用超高效液相色谱（UHPLC）和混合四极杆-Orbitrap高分辨率质谱（Q-Orbitrap HRMS），可以对化妆品中的100种多种受管制成分进行全面鉴定和定量。使用超声辅助萃取（UAE），然后进行分散固相萃取（dSPE），开发了一种简单，高效且便宜的样品预处理方案。通过UHPLC-Q-Orbitrap HRMS在同步全扫描MS和数据相关的MS / MS（全扫描MS ¹ / dd-MS ²）采集模式下分析化妆品样品。对于全扫描MS ¹，质量分辨率设置为70,000 FWHM（半高全宽），对于dd-MS ²，质量分辨率设置为17,500 FWHM对于每个单独的分析物，通过实验测得的准分子离子质量偏差小于2 ppm（百万分之一），特征片段离子的质量偏差小于5 ppm。内部建立了一个精确质量的数据库和一个质谱库，用于搜索100种目标化合物。通过将实验测得的前体离子和碎片离子的准确质量，保留时间，同位素模式和离子比与精确质量数据库进行比较，并将获得的MS / MS质谱图与质谱库进行比对，从而进行了广泛的筛选。根据检测限（LOD），定量限（LOQ），线性，稳定性，准确性和基质效应，对开发的方法进行了评估和验证。