基于UPLC-Q-TOF-MSn的化妆品中40种性激素非法添加分析方法及筛查数据库的建立

Establishment of an Analysis Method and Screening Database for Illegal Addition of 40 Sex Hormones in Cosmetics Based on UPLC-Q-TOF-MS

关键词:  化妆品  非法添加  性激素  超高效液相色谱-飞行时间质谱  筛查数据库

Key words:  cosmetics  illegal addition  sex hormones  UPLC-Q-TOF-MSⁿ  screening database

摘要:

目的 建立基于UPLC-Q-TOF-MSⁿ的化妆品中40种性激素非法添加分析方法及筛查数据库。方法 色谱柱为Agilent SB-C₁₈(2.1 mm×50 mm，1.8 μm)，正离子模式以0.1%甲酸水溶液-乙腈为流动相，负离子模式以水-乙腈为流动相，梯度洗脱，流速0.2 mL·min^-1，柱温35 ℃；采用电喷雾电离源(ESI)，采集模式为Scan MS及Targeted MS/MS，将40种性激素的精确质量数、保留时间、二级质谱图导入PCDL软件建立筛查数据库。结果 采用所建立的数据库方法快速筛查100批化妆品，1批育发类产品检出少量黄体酮。结论 本研究所建立的40种性激素分析方法和筛查数据库具有简便、快速、灵敏和准确的特点，适合化妆品中非法添加性激素的高通量筛查和准确定性。

Abstract:

OBJECTIVE To establish an analysis method and screening database based on UPLC-Q-TOF-MSⁿ for illegal addition of 40 sex hormones in cosmetics. METHODS The gradient elution was carried out on Agilent SB-C₁₈ column (2.1 mm×50 mm, 1.8 μm), 0.1% formic acid water and acetonitrile were used as mobile phase in positive ion mode, water and acetonitrile were used as mobile phase in negative ion mode, the flow rate was 0.2 mL·min^-1, the column temperature was 35℃. MS detection was carried out by electrospray ionization(ESI)mass spectrometer in Scan MS and Targeted MS/MS mode. The accurate mass, retention time and MS/MS mass spectrum of 40 sex hormones were imported into PCDL software to establish a rapid screening database. RESULTS The established method and database was used to screen 100 batches of cosmetics, and one batch of hair-growing product was detected with a small amount of progesterone. CONCLUSION The established analysis method and screening database including 40 sex hormones is fast, sensitive and accurate, which is suitable for high-throughput screening and accurate qualitative analysis of sex hormones adulterants in cosmetics.