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作 者:王红 刘亚蓉 WANG Hong;LIU Ya-rong(Qinghai Institute for Food Control,Xining 810016;Qinghai Institute for Drug Control,Xining 810016)
机构地区:[1]青海省食品检验检测院,西宁810016 [2]青海省药品检验检测院,西宁810016
出 处:《中南药学》2020年第9期1554-1557,共4页Central South Pharmacy
基 金:青海省科技计划项目(编号:2017-ZJ-Y40)。
摘 要:目的提高三味杜鹃汤散的质量标准。方法采用显微鉴别、薄层色谱鉴别对制剂中烈香杜鹃、草豆蔻、干姜进行定性鉴别;以气相色谱法(GC)测定苄基丙酮的含量,采用安捷伦DB-1毛细管柱(长度30 m,内径0.25 mm,膜厚0.25μm);程序升温(初始温度100℃,保持5 min;以5℃·min^-1升温至130℃,保持5 min;再以20℃·min^-1升温至300℃,保持8 min);进样口温度:260℃;检测器温度:310℃;载气:氮气;检测器:FID;线速度:44.9 cm·s^-1;柱流量:1.97 mL·min^-1;分流比:30∶1。结果烈香杜鹃、草豆蔻、干姜显微特征明显易见;烈香杜鹃、草豆蔻的TLC图斑点清晰、分离良好且阴性无干扰;苄基丙酮在0.0541~0.1895μg与峰面积呈良好的线性关系,低、中、高浓度平均加样回收率分别为96.6%,99.9%,97.3%。结论该方法专属性强,准确可靠,能有效控制三味杜鹃汤散的质量。Objective To improve the quality standard of Sanwei Dujuantang powder.Methods Rhododendron anthopogonoides,Alpinia nutmeg and dried ginger were identified by TLC and microscope.The content of benzyl acetone in the preparation was determined by gas chromatography with agilent DB-1 capillary column(length 30 m,inner diameter 0.25 mm,and film thickness 0.25 m).Program heating(initial temperature at 100℃for 5 min,heated to 130℃at 5℃per minute,keeping for 5 min,and then to 300℃at 20℃per minute,keeping for 8 min).The inlet temperature:260℃;the detector temperature:310℃;carrier gas:N2;FID detector;linear speed:44.9 cm·s^-1;column flow rate:1.97 mL·min^-1;and split ratio:30∶1.Results The microscopic characteristics of Rhododendron anthopogonoides,Alpinia nutmeg and dried ginger were obvious.TLC images of Rhododendron anthopogonoides and Alpinia nutmeg showed clear spots,good separation and no interference.The linear relationship of benzyl acetone in 0.0541-0.1895μg was good and the average recovery of low,middle,and high concentration was 96.6%,99.9%,and 97.3%,respectively.Conclusion The method is strongly specific,accurate and reliable,and can effectively control the quality of Sanwei Dujuantang powder.
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