目的 建立气相色谱法(GC)同时测定艾粉中樟脑、异龙脑、L-龙脑、β-石竹烯和花椒油素5个成分含量的方法,并根据含量进行聚类分析。 方法 采用HP-5毛细管柱(30 m×0.32 mm,0.25 μm);升温程序90 ℃保持2 min,以4 ℃·min-1升温至100 ℃,以20 ℃·min-1快速升温至160 ℃,保持6 min;FID检测器温度240 ℃;进样口温度240 ℃;载气高纯氮气,流速3.0 mL·min-1;进样分流比50∶1;进样量0.5 μL。采用SPSS16.0统计软件进行聚类分析。 结果 樟脑、异龙脑、L-龙脑、β-石竹烯和花椒油素分别在0.02～0.32(r=1.000 0),0.01～0.08(r=1.000 0),0.20～7.95(r=1.000 0),0.01～0.40(r=1.000 0),0.08～0.67 mg·mL-1(r=0.999 8)具有良好线性关系,平均加样回收率(n=9)分别为101.04%(RSD 1.04%),99.08%(RSD 1.50%),98.76%(RSD 1.67%),99.85%(RSD 1.97%),97.74%(RSD 1.65%),采用聚类分析能将24批样品按照5个成分的含量聚为3类。 结论 该方法操作简便,快速,准确,重复性和稳定性较好,可为艾粉的多成分测定及其质量评价提供科学依据。
Abstract
OBJECTIVE To establish a GC method for simultaneous determination of camphor, isoborneol, L-borneol, β-caryophyllene and xanthoxylin in aifen, combined with hierarchical cluster analysis. METHODS The GC analysis was carried out on HP-5 capillary column (30 m×0.32 mm, 0.25 μm). Temperature programs:90 ℃ (hold 2 min) programmed to 100 ℃ at 4 ℃·min-1, then programmed to 160 ℃ (hold 6 min) at 20 ℃·min-1. The detector was FID with 240 ℃. The inlet temperature was set at 240 ℃. The carrying gas was high-purity nitrogen (3.0 mL·min-1), split ratio was 50∶1, injection volume was 0.5 μL. Cluster analysis was performed by SPSS16.0 software. RESULTS The methodology validation for the assay of camphor, isoborneol, l-borneol, β-caryophyllene and xanthoxylin presented that they were in good liner correlation in the ranges of 0.02-0.32(r=1.000 0), 0.01-0.08(r=1.000 0), 0.20-7.95(r=1.000 0), 0.01-0.40(r=1.000 0), 0.08-0.67 mg·mL-1(r=0.999 8), with the average recoveries (n=9) of 101.04% (RSD=1.04%), 99.08%(RSD=1.50%), 98.76% (RSD=1.67%), 99.85%(RSD=1.97%), 97.74% (RSD=1.65%), respectively. The 24 batches of sample analyzed can be clustered into three classes according to the content of the five components. CONCLUSION The developed method is simple, quick and accurate, which provides reference for the quality control of aifen.
关键词
艾粉 /
樟脑 /
异龙脑 /
L-龙脑 /
β-石竹烯 /
花椒油素 /
含量测定 /
聚类分析
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Key words
aifen /
camphor /
isoborneol /
l-borneol /
β-caryophyllene /
xanthoxylin /
content determination /
cluster analysis
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中图分类号：
R284
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参考文献
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脚注
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基金
国家自然科学基金资助项目(81374065);黔科合重大专项字(6011)
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