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纸质出版日期:2009
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刘东辉1, 陈慕媛1, 黄月纯2, 等. 双柏散中槲皮苷与薄荷脑的含量测定研究[J]. 中国实验方剂学杂志, 2009,15(12):4-7.
LIU Dong-hui1, CHEN Mu-yuan1, HUANG Yue-chun2, et al. Determination of Quercitrin and Menthol in Shuangbaisan[J]. Chinese journal of experimental traditional medical formulae, 2009, 15(12): 4-7.
目的:建立双柏散中槲皮苷和薄荷脑的含量测定方法
为双柏制剂的质量控制与化学物质基础研究提供分析手段。方法:采用HPLC法测定槲皮苷含量。采用Eclipse XDB C18为色谱柱;流动相为乙腈-0.01mol·L-1磷酸二氢钾溶液-冰醋酸(16∶84∶2.1);检测波长为352nm;流速为1mL·min-1;柱温为40℃。以水杨酸甲酯为内标物
采用GC法测定薄荷脑的含量。以HP-5为色谱柱
进样口温度为210℃;FID检测器
检测器温度为280℃
程序升温:初始温度50℃
保持2min后
以60℃·min-1升至120℃后保持5min
再以10℃·min-1升至150℃后
再以60℃·min-1升至235℃后保持10min;流速为1.1mL·min-1
分流比为1∶1。结果:槲皮苷在0.02048~1.2288μg范围内线性关系良好(r=0.9999)
平均加样回收率为97.20%(RSD=1.75%);薄荷脑在0.00273~0.08736μg范围内线性关系良好(r=0.9995)
平均加样回收率为99.97%(RSD=2.88%)。双柏散中槲皮苷、薄荷脑含量分别为0.8519~1.2863mg.g-1、0.0683~0.8556mg.g-1。结论方法简便、重复性好
为双柏制剂的质量控制与化学物质基础研究提供了一定的分析手段。
Objective:To establish a method for the determination of quercitrin and menthol in Shuangbaisan
and provide a reference for quality control and the chemical material foundation of Shuangbai preparations.Methods:The content of the quercitrin was determined by HPLC.Eclipse XDB C18 was used
with acetonitrile-0.01 mol·L-1 potassium dihydrogen phosphate-acetic acid(16∶84∶2.1)as a mobile phase
detection wavelength at 352nm
flow rate at 1mL·min-1
and column temperature at 40 ℃.With Borneolum syntheticum as the internal standard
GC with HP-5 column was used
sampling temperature at 210℃
FID detector temperature at 280℃
temperature programming started at 50 ℃
held for 2 min
increased at a rate of 60 ℃·min-1 to 120 ℃
held for 5 minites
increasd at a rate of 10 ℃·min-1 to 150 ℃
then increased at a rate of 60 ℃·min-1 to 235 ℃ and kept it for 10 minites
low rate at 1.1 mL·min-1
spilt ratio was 1∶1.Results: Good linearity for Quercitrin and Menthol were in the rang of 0.020 48~1.228 8 μg(r>=0.999 9) and 0.002 73~0.087 36 μg(r>=0.999 5)
respectively.The average recoveries were 97.20%(RSD=1.75 %) for quercitrin and 99.97%(RSD=2.88%[0]) for menthol.The concents of quercitrin and menthol in Shuangbaisan were 0.851 9~1.286 3 mg·g-1、0.068 3~0.855 6 mg·g-1
respectively. Conclusion:This method is reliable and simple
which provides a reference for the quality control of Shuangbaisan.
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