PMID- 35362682 OWN - NLM STAT- MEDLINE DCOM- 20220404 LR - 20220915 IS - 1872-2059 (Electronic) IS - 1000-8713 (Print) IS - 1000-8713 (Linking) VI - 40 IP - 4 DP - 2022 Apr TI - [Determination of 19 illegally added chemical ingredients in hair loss prevention cosmetics by ultra-performance liquid chromatography-quadrupole-time of flight mass spectrometry]. PG - 343-353 LID - 10.3724/SP.J.1123.2021.08019 [doi] AB - Cosmetic products for hair loss prevention are often mixed with prohibited substances such as hormones, antibiotics, and forbidden pharmacologically active substances. Although drugs increase the efficacy of cosmetic products, they cause skin irritation and allergic reactions, upon long-term exposure. Given the increasing number of hair loss prevention cosmetics on the market, the need to guarantee product safety calls for efficient and reliable methods to identify illegal ingredients in these products. Chromatography combined with high-resolution mass spectrometry offers the advantages of high resolution and high throughout, thus being a powerful technique for simultaneously detecting illegal ingredients in cosmetics. In this study, an ultra-performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF-MS) method for detecting 19 illegal chemical components was established. Combined with the scientific database, a screening platform for hair loss prevention cosmetics was constructed. The effect of extraction solvent was investigated. The chromatographic and mass spectrometry conditions were optimized. Under the optimal conditions, separation was achieved within 20 min on an ACQUITY UPLC BEH C18 column (100 mmx2.1 mm, 1.7 mum). Acetonitrile and 2 mmol/L ammonium formate solution containing 0.05% formic acid were used as mobile phases for gradient elution. The 19 compounds were detected by positive ion electrospray ionization (ESI) in the MS(E) mode. The chromatographic retention time, precursor ions, product ions of the target analytes, and abundance ratio were collected to construct a screening database with UNIFI software. The 19 compounds were well separated, with good linearity. The limits of detection (LODs) and limits of quantification (LOQs) were 0.025-0.05 mug/g and 0.075-0.15 mug/g, respectively. Hair lotion and shampoo, which are commonly marketed as hair loss prevention cosmetics, were selected as the respective matrices for the recovery experiment. The average recoveries of the 19 compounds ranged from 68.6% to 118.6%, and the relative standard deviations (RSDs) were 0.3%-10.3%. Then, 77 batches of cosmetic samples were detected and screened under the same conditions. The TOF-MS information, including the retention time, ion addition mode, mass-to-charge ratio of the parent ions and fragment ions, as well as the abundance ratio, were compared between the cosmetic samples and the standard MS information with UNIFI software. Finally, two batches of samples that were illegally adulterated with minoxidil and finasteride were identified. The ESI fragmentation pathway of the product ions from minoxidil was also proposed. The matrix matching external standard method was used to determine the amounts of minoxidil and finasteride in the two batches of hair lotion, and they were as high as 60 mg/g and 0.31 mg/g, respectively. This result revealed that multiple chemical components were simultaneously added to hair loss prevention cosmetics. Furthermore, the amount of the illegally added drug was very high, indicating high safety risk for consumers using such cosmetics. The present method has the advantages of simple operation, high sensitivity, and good reproducibility. It can be used for rapid screening and simultaneous quantitative analysis of various illegal chemicals in hair loss prevention cosmetics. FAU - Dong, Yalei AU - Dong Y AD - National Institutes for Food and Drug Control, Key Laboratory for Researching and Evaluation of Cosmetics of National Medical Products Administration, Beijing 100050, China. FAU - Niu, Shuijiao AU - Niu S AD - Shandong Institute for Food and Drug Control, Jinan 250101, China. FAU - Qiao, Yasen AU - Qiao Y AD - National Institutes for Food and Drug Control, Key Laboratory for Researching and Evaluation of Cosmetics of National Medical Products Administration, Beijing 100050, China. FAU - Huang, Chuanfeng AU - Huang C AD - National Institutes for Food and Drug Control, Key Laboratory for Researching and Evaluation of Cosmetics of National Medical Products Administration, Beijing 100050, China. FAU - Wang, Haiyan AU - Wang H AD - National Institutes for Food and Drug Control, Key Laboratory for Researching and Evaluation of Cosmetics of National Medical Products Administration, Beijing 100050, China. FAU - Sun, Lei AU - Sun L AD - National Institutes for Food and Drug Control, Key Laboratory for Researching and Evaluation of Cosmetics of National Medical Products Administration, Beijing 100050, China. LA - chi PT - Journal Article PL - China TA - Se Pu JT - Se pu = Chinese journal of chromatography JID - 9424804 RN - 0 (Cosmetics) RN - 0 (Hair Preparations) SB - IM MH - Alopecia/prevention & control MH - Chromatography, High Pressure Liquid MH - Chromatography, Liquid MH - *Cosmetics/analysis MH - *Hair Preparations MH - Humans MH - Reproducibility of Results MH - Tandem Mass Spectrometry PMC - PMC9404028 OTO - NOTNLM OT - hair loss prevention cosmetics OT - high resolution mass spectrometry (HRMS) OT - illegally added OT - screening OT - ultra-performance liquid chromatography (UPLC) EDAT- 2022/04/02 06:00 MHDA- 2022/04/05 06:00 PMCR- 2022/04/08 CRDT- 2022/04/01 08:40 PHST- 2022/04/01 08:40 [entrez] PHST- 2022/04/02 06:00 [pubmed] PHST- 2022/04/05 06:00 [medline] PHST- 2022/04/08 00:00 [pmc-release] AID - 1000-8713-40-4-343 [pii] AID - 10.3724/SP.J.1123.2021.08019 [doi] PST - ppublish SO - Se Pu. 2022 Apr;40(4):343-353. doi: 10.3724/SP.J.1123.2021.08019.