[关键词]
[摘要]
目的 建立红核妇洁洗液GC指纹图谱,并同时测定其中9种成分的含量。方法 采用DB-5毛细管柱(30 m×0.32 mm,1.5 μm),程序升温,以愈创木酚为参照峰,建立20批样品的GC指纹图谱,同时测定糠醛、5-酮基己腈、愈创木酚、5-甲基愈创木酚、4-甲基愈创木酚、3-甲氧基邻苯二酚、4-乙基愈创木酚、2,6-二甲氧基苯酚、2,6-二甲氧基-4-甲基苯酚的含量。结果 建立了红核妇洁洗液GC指纹图谱,共标定13个共有峰,20批样品相似度均在0.90以上,精密度、重复性和稳定性试验中相对保留时间和相对峰面积的RSD值均小于2%。其中糠醛、5-酮基己腈、愈创木酚、5-甲基愈创木酚、4-甲基愈创木酚、3-甲氧基邻苯二酚、4-乙基愈创木酚、2,6-二甲氧基苯酚和2,6-二甲氧基-4-甲基苯酚分别在0.059 7~5.966 6 μg、0.004 6~0.463 7 μg、0.017 4~1.736 6 μg、0.004 1~0.409 9 μg、0.013 9~1.386 4 μg、0.006 5~0.645 5 μg、0.007 5~0.746 7 μg、0.021 8~2.181 9 μg和0.017 1~1.710 6 μg进样量与色谱峰峰面积呈良好线性响应;平均回收率分别为99.9%、98.8%、99.6%、99.3%、99.6%、99.4%、99.3%、99.5%、99.0%;RSD分别为0.07%、0.41%、0.18%、0.72%、0.37%、0.62%、0.44%、0.48%、0.52%。20批样品中糠醛、5-酮基己腈、愈创木酚、5-甲基愈创木酚、4-甲基愈创木酚、3-甲氧基邻苯二酚、4-乙基愈创木酚、2,6-二甲氧基苯酚和2,6-二甲氧基-4-甲基苯酚的质量浓度分别为5.376~6.265 mg/mL、0.418~0.487 mg/mL、1.565~1.824 mg/mL、0.369~0.431 mg/mL、1.248~1.455 mg/mL、0.582~0.678 mg/mL、0.673~0.784 mg/mL、1.966~2.291 mg/mL、1.541~1.797 mg/mL。结论 该方法简单、准确、重复性好,可用于红核妇洁洗液的质量控制和评价。
[Key word]
[Abstract]
Objective To establish the GC fingerprint of Honghe Fujie Lotion (HFL) and determine the content of nine constituents. Methods The analysis of HFL was performed on a column of DB-5 capillary column (30 m×0.32 mm, 1.5 μm) with temperature programming, the GC fingerprint of 20 batches of samples were established with guaiacol as a reference peak; And the content of furfural, 5-ketohexonitrile, guaiacol, 5-methylguaiacol, 4-methylguaiacol, 3-methoxycatechol, 4-ethylguaiacol, and 2,6-dimethoxy phenol and 2,6-dimethoxy-4-methylphenol was determined. Results The GC fingerprint of HFL was set up with 13 common peaks, and the similar degrees of all samples were over 0.90, the RSD values of relative retention time and relative peak area in precision, repeatability and stability tests were all less than 2%. The linear ranges of furfural, 5-ketohexonitrile, guaiacol, 5-methylguaiacol, 4-methylguaiacol, 3-methoxycatechol, 4-ethylguaiacol, 2,6-dimethoxy phenol, and 2,6-dimethoxy-4-methylphenol fell within the range of 0.059 7-5.966 6 μg, 0.004 6-0.463 7 μg, 0.017 4-1.736 6 μg, 0.004 1-0.409 9 μg, 0.013 9-1.386 4 μg, 0.006 5-0.645 5 μg, 0.007 5-0.746 7 μg, 0.021 8-2.181 9 μg, and 0.017 1-1.710 6 μg, respectively. The recoveries were 99.9%, 98.8%, 99.6%, 99.3%, 99.6%, 99.4%, 99.3%, 99.5%, and 99.0%, respectively. The relative standard deviations were 0.07%, 0.41%, 0.18%, 0.72%, 0.37%, 0.62%, 0.44%, 0.48%, and 0.52%, respectively. The content of twenty samples of furfural, 5-ketohexonitrile, guaiacol, 5-methylguaiacol, 4-methylguaiacol, 3-methoxycatechol, 4-ethylguaiacol, 2,6-dime-thoxy phenol, and 2,6-dimethoxy-4-methylphenol was 5.376-6.265, 0.418-0.487, 1.565-1.824, 0.369-0.431, 1.248-1.455, 0.582-0.678, 0.673-0.784, 1.966-2.291, 1.541-1.797 mg/mL. Conclusion The established method is simple, accurate, and reproducible, which can be used for the quality control and evaluation of HFL.
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[基金项目]
山东省自然科学基金资助项目(ZR2013HM074)