摘要
建立了测定三种香豆素类物质——香豆素,6-甲基香豆素,7-甲氧基香豆素——在化妆品中含量的气相色谱质谱法。采用甲醇超声提取,气相色谱法分离测定。色谱柱为HP-5柱,流动相为高纯氮气,流速为1.5ml/min,分流比为10∶1,气化室温度为240℃,程序升温,初温100℃,保留1min,以5℃/min的速率升至120℃,继续以20℃/min的速率升至250℃,保留1min。总分析时长12.5min。检测器温度为280℃。结果为三种被测物在1～50μg/mL范围内均与对应的峰面积呈良好线性关系(r>0.9999)。在添加浓度为1.1,2.0,5.0μg/mL时,回收率在90.0%～102.8%之间,精密度RSD<2.7,最低检出限为香豆素0.3μg/mL(S/N=3.0),6-甲基香豆素0.3μg/mL(S/N=3.2),7-甲氧基香豆素0.5μg/mL(S/N=5.0)。最后使用质谱进行验证。该法简便、快速、准确,可用于化妆品中的此三种物质含量的检测。
Three cournarins - coumarin, 6-methyl coumarin, 7-methoxy coumarin - in cosmetics were simultaneously determined by gas chromatography（GC） and mass spectrometry（MS）. The cosmetics were extracted with methanol using a sonieator, centrifuged and filtered. Filtrates were analyzed by GC. The samples were separated with HP-5 column with a gas flow rate of 1.5ml/min and programming column temperature. The initial temperature was set at 100℃ for 1 min, then 5℃/min to 120℃, and 20℃/min to 250℃ for lmin. The total time was 12.5min. The calibration curves of 3 eoumarin compounds were linear（r〉0.9999） between 1-50 μg/mL. The precision was perfect （RSD〈2.7）.The average recoveries were from 90.0% to 102.8%. The detection limit was 0.3 μg/mL of coumarin （S/ N=3.0）, 0.3 μg/mL of 6-methyl coumarin （S/N=3.2）and 0.5 μg/mL of 7-methoxy coumarin （S/N=5.0）. The suspected samples will be confirmed by mass spectrometry then. The method is simple and quick with high accuracy, and it is suitable for the determination of coumarin compounds in cosmetics.
出处
《生命科学仪器》
2006年第1期33-36,共4页
Life Science Instruments
