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目的建立3种不同性状化妆品中甲醛的快速、准确的检测方法。方法采用静态顶空结合GC-MS法,水剂、乳液、膏状物化妆品顶空加热平衡温度分别为50℃、60℃、70℃,加热平衡时间为15 min,色谱柱为CD-624毛细管柱(60 m×0.32 mm,1.8μm),柱温为40℃保持2 min,10℃/min升至260℃,保持1 min;进样口温度为240℃,分流比为5∶1,氦气流速为1 ml/min,离子源温度为230℃,传输线温度为280℃,电离能量70 e V,SIM数据采集模式,定量离子为m/z 30。结果甲醛浓度为10 mg/kg~200 mg/kg时,线性相关性良好(r=0.999 6)。3种浓度系列溶液测定结果的相对标准偏差(RSD)为1.02%~1.42%,回收率为85.5%~104.2%,以3倍信噪比(S/N=3)计算得出方法的最低检出限为1.25 mg/kg。结论方法简便可行,检测灵敏度、准确度及精密度均可满足化妆品中甲醛含量的检测要求。
Objective To establish a rapid and accurate method for the determination of formaldehyde in three different cosmetic traits. Methods The static headspace coupled GC-MS method was used. The headspace equilibrium temperatures of cosmetics, lotions and creams were 50 ℃, 60 ℃ and 70 ℃ respectively. The heating time was 15 min. The column was CD-624 capillary Column (60 m × 0.32 mm, 1.8 μm). The column temperature was maintained at 40 ℃ for 2 min and the temperature was raised to 260 ℃ at 10 ℃ / min for 1 min. The inlet temperature was 240 ℃ and the split ratio was 5:1. Gas flow rate of 1 ml / min, ion source temperature of 230 ℃, transmission line temperature of 280 ℃, ionization energy 70 e V, SIM data acquisition mode, quantitative ions m / z 30. Results When the concentration of formaldehyde was 10 mg / kg ~ 200 mg / kg, the linear correlation was good (r = 0.999 6). The relative standard deviations (RSDs) were 1.02% ~ 1.42% and the recoveries were 85.5% ~ 104.2% for the three concentration series of solutions. The lowest detection limit was obtained by 3 times signal to noise ratio (S / N = 3) The limit is 1.25 mg / kg. Conclusion The method is simple and feasible, and the detection sensitivity, accuracy and precision can meet the requirements of formaldehyde content in cosmetics.