气相色谱法测定斑贴膜片中香料混合物含量的研究

Determination of the Fragrance Mixtures in Patch Paster by Capillary Gas Chromatography

关键词:  气相色谱法  香料  斑贴膜片  IV型变态反应

Key words:  gas chromatography  fragrance mixtures  patch paster  type IV allergy

摘要:

目的 建立毛细管气相色谱法测定用于检测IV型变态反应的斑贴膜片中7种香料混合物(香叶醇、羟基香茅醛、桂皮醛、丁香酚、戊基桂皮醛、桂皮醇、异丁香酚)含量的方法。方法 每片膜片用1 mL乙醇提取30 min，提取液直接注入气相色谱分析，采用极性PEG-20M毛细管气相色谱柱分离，外标法定量。结果 7种香料组份的线性关系良好(r≥0.999 5)；精密度和稳定性试验 RSD(n=8)均<2%；加标回收率范围95.48%~107.52%, RSD 0.31%~2.00%；贴片香料含量均匀性试验 RSD(n=8)<5% ；定量限分别为3.7，4.3，3.3，3.5，2.8，2.3，2.9 μg·mL^-1。结论 本方法样品前处理简单，分析快速、准确和灵敏，可满足斑贴膜片中香料混合物定量检测的需要。

Abstract:

OBJECTIVE To establish a method for the determination of the mixtures of seven fragrance ingredients, including geraniol, hydroxy citronellal, cinnamaldehyde, eugenol, amylcinnamic aldehyde, cinnamyl alcohol and isoeugenol，in patch paster which can be used for testing type IV allergy by capillary gas chromatography. METHODS Each patch was extracted with 1 mL ethanol for 30 minutes. The extraction liquid was injected into GC for separation with a polar PEG-20M capillary column. The external standard method was used for quantitative analysis. RESULTS The standard curves were linear on a certain concentration with correlation coefficients larger than 0.999 5 for the seven target fragrances. The relative standard deviations (n=8) of precision and stability were less than 2%. The average recoveries for seven fragrances were between 95.48% and 107.52% with RSD(n=3) in the range of 0.31%~2.00%. The relative standard deviations (n=8) of uniformity were less than 5%. The quantitative limits for seven fragrances were 3.7, 4.3, 3.3, 3.5, 2.8, 2.3, 2.9 μg·mL^-1 respectively. CONCLUSION This method is simple, rapid, sensitive and accurate. It could meet the requirement for the quantitative analysis of fragrance ingredients in patch paster.