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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3.7,4.3,3.3,3.5,2.8,2.3,2.9μg.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。
OBJECTIVE To establish a capillary gas chromatographic method for the determination of seven kinds of flavoring mixtures (geraniol, hydroxycitronellal, cinnamaldehyde, eugenol, amylcinnamide, cinnamyl alcohol, isoeugenol ) Content of the method. Methods Each membrane was extracted with 1 mL of ethanol for 30 min. The extract was directly injected into gas chromatographic analysis and separated by polar PEG-20M capillary gas chromatographic column with external standard method. Results The linearity of the seven components was good (r≥0.999 5). The RSD (n = 8) of the precision and stability tests were all less than 2%. The spiked recoveries ranged from 95.48% to 107.52% and RSD from 0.31% to 2.00 %; Patch content uniformity test RSD (n = 8) <5%; The limit of quantification were 3.7,4.3,3.3,3.5,2.8,2.3,2.9μg.mL 1. Conclusion The method of sample pretreatment is simple, rapid, accurate and sensitive analysis, which can meet the needs of the quantitative detection of the spice mixture in patch film.