摘要
为建立消喘贴敷膏剂的质量控制方法,本文采用薄层色谱法对消喘贴敷膏剂中的白芥子、延胡索、细辛、荜茇进行定性分析。采用高效液相色谱法对白芥子的芥子碱硫氰酸盐进行含量测定,色谱柱为Phenomenex Geminin C18色谱柱(150 mm×4.6 mm,5μm),以乙腈-0.08 mol/L磷酸二氢钾溶液(13∶87,V/V)为流动相,检测波长326 nm,流速1.0 m L/min,柱温25℃,进样量20μL。鉴定结果表明,4味中药斑点清晰,分离较好,阴性对照无干扰。芥子碱硫氰酸盐在0.84~8.4μg范围内呈良好的线性关系(r=0.999 7),平均加样回收率(n=6)为99.58%(相对标准偏差为0.37%)。该方法简单快捷、准确可靠,专属性强,可用于消喘贴敷膏剂的质量控制。
To establish the quality control method of Xiaochuan Emplastrum,Sinapis Semen, Corydalis Rhizoma, Asari Radix et Rhizoma and Piperis Longi Fructus in the Xiaochuan Emplastrum were qualitatively analyzed by TLC. The content of sinapine thiocyanate in sinapis semen was determined by HPLC. The chromatographic column was Phenomenex Geminin C18 column（150 mm×4.6 mm, 5 μm）. The mobile phase was acetonitrile0.08 mol/L potassium phosphate monobasic （13∶87,V/V） at the flow rate of 1.0 mL/min, the detection wavelength of 326 nm, the column temperature of 25 ℃ and the sample volume of 20 μL. The results revealed that the spots in the TLC identification of Sinapis Semen, Corydalis Rhizoma, Asari Radix et Rhizoma and Piperis Longi Fructus were clear, well separated and without interference by the negative control. The calibration curve of sinapine thiocyanate showed good linearity in the range of 0.84～8.4 μg （r=0.999 7）. The average recovery was 99.58 % （n=6,reltive standard deviatior is 0.37 %）. This method is rapid, accurate, reliable, and specific, thus it can be used for the effective quality control of the Xiaochuan Emplastrum.
出处
《山东科学》
CAS
2017年第3期39-44,共6页
Shandong Science
基金
青岛市2015-2016年度中医药科研计划(2015-zyy012)
