摘要
目的 建立十一味草果丸气相色谱法(GC)指纹图谱,并测定其中桉油精、丁香酚、土木香内酯、异土木香内酯、去氢木香内酯的含量.方法 采用SH-WAX(0.25 mm × 0.25 µm×30m)毛细管柱;进样口温度为220℃;检测器温度为240℃;程序升温;分流比为10∶1.结果 建立了 10批十一味草果丸指纹图谱,相似度均大于0.99,共标定了 20个共有峰,对其中5个成分(桉油精、丁香酚、土木香内酯、异土木香内酯、去氢木香内酯)进行含量测定,各成分质量浓度分别在 0.80～7.98 μg·mL-1,34.93～349.30 μg·mL-1,19.66～196.57 µg·mL-1,23.44～234.39 μg·mL-1,14.21～142.14 µg·mL-1 内与峰面积呈良好的线性关系(r≥0.9998);高、中、低浓度的平均加样回收率(n=3)分别在90.68％～92.66％、95.44％～96.42％、99.59％～102.38％、98.34％～103.04％、98.94％～101.66％.结论 建立的指纹图谱及多成分含量测定方法专属性强、精密度高、稳定可靠,可较为全面地对十一味草果丸进行质量控制,为其质量评价和标准建立提供科学依据.
Abstract
Objective To establish the gas chromatographic(GC)fingerprints of Shiyiwei Caoguo pills and to determine the content of eucalyptus oleoresin,eugenol,geomannan lactone,isogeomannan lactone and dehydrogeomannan lactone.Methods SH-WAX(0.25 mm × 0.25 μm×30 m)capillary column was used.The temperature of the injection port was 220 ℃;the temperature of the detector was 240 ℃;the column temperature was programmed to increase;and the partition ratio was 10∶1.Results The fingerprints of 10 batches of Shiyiwei Caoguo pills were established,with similarities all greater than 0.99.Totally 20 common peaks were calibrated,and the content of 5 components(eucalyptus oleoresin,eugenol,geomannanolide lactone,isogeomannanolide lactone,and dehydrogeomannanolide lactone)were determined.The linearity concentrations ranged 0.80～7.98 μg·mL-1,34.93～349.30μg·mL-1,19.66～196.57 μg·mL-1,23.44～234.39 μg·mL-1 and 14.21～142.14 μg·mL-1,respectively(r≥0.9998).The average recoveries of low,middel,high concentration(n=3)were within 90.68％～92.66％,95.44％～96.42％,99.59％～102.38％,98.34％～103.04％,and 98.94％～101.66％.Conclusion The established fingerprints and multi-component content determination methods are exclusive,stable and reliable,which can be used to control the quality of Shiyiwei Caoguo pills comprehensively,and provide a scientific basis for the quality control and standards establishment.
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