摘要
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 A rapid and accurate method was developed for the determination of formaldehyde in three types of cosmetic products. Methods Headspace and GC-MS were employed for the analysis of formaldehyde in 3 types of cosmetic products. The optimal conditions were that equilibrium temperature was 50 ℃,60 ℃,70 ℃ for water-based,emulsion and paste cosmetic products respectively; equilibrium time was 15 min; chromatographic column was CD-624（ 60 m × 0. 32 mm,1. 8μm）,with column temperature of 40 ℃ for 2 min,10 ℃ /min to 260 ℃ for 1 min; injection temperature was 240 ℃; split ratio was 5∶1; He flow rate was 1 ml / min; EI source temperature was 230 ℃; transmission line temperature was 280 ℃; ionization energy was 70 e V; data acquisition mode was SIM; and quantitative ion was m / z 30. Results The results showed that the correlation coefficient（ r） was 0. 999 6 when the concentration of it was among 10 mg / kg-200 mg / kg,with the RSD of1. 02%-1. 42% for three concentration series,and the recovery rate of among 85. 5%-104. 2%. The detection limit of formaldehyde was 1. 25 mg / kg calculated by three times of the S / N. Conclusion The method is applicable,and the sensitivity,accuracy and prevision all meet the analysis requirement.
出处
《中国卫生检验杂志》
CAS
2015年第23期4013-4014,4018,共3页
Chinese Journal of Health Laboratory Technology
关键词
静态顶空
气相色谱-质谱联用法
化妆品
甲醛
Headspace
Gas chromatography-mass spectrometry
Cosmetic products
Formaldehyde
