一测多评法同时测定止痢宁片中4个萜类内酯的含量

目的:建立采用一测多评法测定止痢宁片中4个萜类内酯含量的分析方法,验证该方法的可行性。方法:采用Kromasil C₁₈色谱柱(250 mm×4.6 mm,5 μm),以甲醇(A)-水(B)为流动相,梯度洗脱(0~60 min,45%A→80%A),流速1.0 mL·min^-1,检测波长225 nm(0~24 min,检测穿心莲内酯;33~60 min,测木香烃内酯和去氢木香内酯)、250 nm(24~33 min,检测脱水穿心莲内酯);以脱水穿心莲内酯为内标,建立穿心莲内酯、木香烃内酯和去氢木香内酯间的相对校正因子,分别采用一测多评法和外标法测定止痢宁片中4个萜类内酯的含量,比较一测多评法计算值与外标法实测值的差异。结果:在一定的线性范围内,穿心莲内酯、木香烃内酯和去氢木香内酯与脱水穿心莲内酯间的相对校正因子分别为0.872、1.424和1.337,一测多评法计算值与外标法实测值之间没有显著性差异,所得的相对校正因子可信。结论:一测多评法质量评价模式可用于止痢宁片中4个萜类内酯的含量测定。

Objective:To establish a quality evaluation method for quantitative analysis of multi-components with a single marker(QAMS)so as to simultaneously determine the contents of four terpene lactones in Zhilining tablets.Methods:The Kromasil C₁₈ column(250 mm×4.6 mm, 5 μm)was adopted.The mobile phase consisted of methanol(A)-water(B)with gradient elution(0-60 min,45%A→80%A)at a flow rate of 1.0 mL·min^-1.The detection wavelengths were changeable(0-24 min,225 nm for detection of andrographolide; 33-60 min, 225 nm for detection of costunolide and dehydrocostuslactone; 24-33 min, 250 nm for detection of dehydroandrographolide).Dehydroandrographolide was used as the internal reference substance.The relative correlation factors(RCFs)of andrographolide, costunolide, and dehydrocostuslactone to dehydroandrographolide were calculated and established.The contents of these four terpene lactones were determined by the external standard method(ESM)and QAMS method, respectively.The QAMS method was validated through comparison of the results obtained by the two different methods.Results:The values of RCFs of andrographolide, costunolide, and dehydrocostuslactone to dehydroandrographolide were 0.872, 1.424 and 1.337 respectively.The two methods did not show significant difference in assay results and the RCFs were reliable.Conclusion:The QAMS method is feasible, accurate, and can be used to determine four terpene lactones in Zhilining tablets.