Abstract：
Recently, many new types of cosmetic illegal additives have been screened in the market. Most of the new additives were new drugs or analogues with very similar structures to other prohibited additives, which were difficult to be identified by liquid chromatography-mass spectrometry (LC-MS) only. Therefore, a new strategy is proposed, which is chromatographic separation combined with nuclear magnetic resonance spectroscopy (NMR) structural identification. The suspected samples were screened by ultra-high-performance liquid chromatography tandem high-resolution mass spectrometry (UPLC-Q-TOF-MS), followed by purification and extraction through silica-gel column chromatography and preparative high-performance liquid chromatography (HPLC). Finally, the extracts were identified unambiguously by NMR as bimatoprost and latanoprost, which were identified to be new cosmetic illegal additives in eyelash serums in China. Meanwhile, bimatoprost and latanoprost were quantified by high-performance liquid chromatography tandem triple quadrupole mass spectrum (HPLC-QQQ-MS/MS). The quantitative method demonstrated good linearity in the range of approximately 0.25-50 ng/mL (R2 > 0.9992), with limit of detection (LOD) and limit of quantification (LOQ) values of 0.01 and 0.03 mg/kg, respectively. The accuracy, precision, and reproducibility were confirmed to be acceptable.
摘要：
最近,市场上已经筛选了许多新型的化妆品非法添加剂。大多数新添加剂是新药或类似物，与其他违禁添加剂的结构非常相似，仅通过液相色谱-质谱（LC-MS）难以鉴定。因此,提出了新的战略，这是色谱分离结合核磁共振波谱（NMR）结构鉴定。通过超高效液相色谱串联高分辨质谱(UPLC-Q-TOF-MS)筛选可疑样品,然后通过硅胶柱色谱和制备型高效液相色谱（HPLC）纯化和萃取。最后,通过NMR明确鉴定提取物为比马前列素和拉坦前列素，在中国被确定为睫毛血清中的新型化妆品非法添加剂。同时,采用高效液相色谱串联三重四极杆质谱(HPLC-QQQ-MS/MS)定量比马前列素和拉坦前列素。定量方法在约0.25-50ng/mL范围内表现出良好的线性（R2>0.9992），检测限（LOD）和定量限（LOQ）值为0.01和0.03mg/kg，分别。准确性,精度,和重现性被证实是可以接受的。
