藏药八味秦皮丸中秦皮甲素、秦皮乙素和麝香酮的定量测定

Determination of aesculin,aesculetin and muscone in Bawei Qinpi Pill

目的建立八味秦皮丸(秦皮、针铁矿、草莓、多刺绿绒蒿、寒水石、美丽风毛菊、朱砂、麝香)质量标准中的定量测定项。方法采用高效液相色谱法测定秦皮甲素和秦皮乙素,色谱柱为依利特C18柱(4.6mm×250mm);流动相为甲醇-0.1%磷酸溶液(27∶73);体积流量为1.0 mL/min;柱温为室温;检测波长为344.4 nm。采用气象色谱法测定麝香酮,色谱柱为HP-5毛细管柱(30 m×0.25 mm×0.25μm);载气为氮气(99.99%);检测器温度为250℃;分流比为40∶1;程序升温150℃开始以10℃/min速度升温至170℃保持4 min,然后以15℃/min速度升温至230℃保持5 min。结果秦皮甲素、秦皮乙素进样量分别在0.200～2.502μg、0.120～1.503μg范围内线性关系良好(r=0.999 9),平均回收率分别为100.71%、100.38%,RSD分别为0.65%、0.87%(n=6);麝香酮进样量在15.20～152.0μg范围内线性关系良好(r=0.999 9),平均回收率为99.27%,RSD为0.74%(n=6)。结论该方法灵敏、准确、专属性强,可用于八味秦皮丸中秦皮甲素、秦皮乙素、麝香酮的定量测定。

AIM To establish the determination methods for aesculin,aesculetin and muscone in Bawei Qinpi Pill（Fraxini Cortex,Goethite,Fragaria orientalis Lozinsk,Meconopsis horridula Hook.f.ex Thoms.,Gypsum,Saussurea superba Anthony f.Pygmaea Anthony,Cinnabaris,Moschus）.METHODS Aesculin and aesculetin in Bawei Qinpi Pill were determined by HPLC.The sample was separated on Elite C18column（4.6 mm×250 mm） using methano1-0.1% phosphoric acid（27∶ 73） as a mobile phase at the flow rate of 1.0 mL/min.The column tempe-rature was room temperature and the detection wavelength was set at 344.4 nm.Muscone in Bawei Qinpi Pill was determined by GC on the column of HP-5（30 m×0.25 mm×0.25 μm）;carrier gas was nitrogen（99.99%）;the detector temperature was at 250 ℃;injector temperature was at 220 ℃;split ratio was 40∶ 1;the initial temperature was started at 150 ℃ and raised to 170 ℃ at the speed of 10 ℃/min and maintained for 4 min,then the temperature was raised to 230 ℃ at the speed of 15 ℃/min and maintained for 5 min.RESULTS The linear ranges of aesculin and aesculetin fell within 0.200-2.502 μg and 0.120-1.503 μg（r=0.999 9）;the average recoveries were 100.71% and 100.38% respectively（RSD was 0.65%,n=6）.The linear range of muscone fell within 15.20-152.0 μg（r=0.999 9） and the average recovery was 99.27%（RSD was 0.87%,n=6）.CONCLUSION The method is sensitive,accurate and specific and can be used to determine aesculin,aesculetin and muscone in Bawei Qinpi Pill.