一测多评法测定利胆排石片中木香内酯类成分的含量

目的：建立一测多评法测定利胆排石片中木香烃内酯和去氢木香内酯的含量。方法：采用UPLC法，使用Acquity UPLC BEH C₁₈色谱柱（2.1 mm×50 mm，1.7 μm），流动相为甲醇-水（50：50），流速0.3 mL·min^-1，柱温40 ℃，检测波长225 nm；以木香烃内酯为内标，建立其与去氢木香内酯的相对校正因子，用UPLC法进行含量测定，计算木香烃内酯、去氢木香内酯的含量，对一测多评法的计算值与外标法实测值进行比较。结果：木香烃内酯、去氢木香内酯线性范围分别为0.028~0.42 μg（r=0.999 9）和0.014~0.21 μg（r=0.999 9），精密度RSD分别为1.0%和0.63%，重复性RSD分别为1.0%和1.4%，平均加样回收率（n=6）分别为100.5%（RSD=1.6%）和99.5%（RSD=2.5%）。去氢木香内酯对木香烃内酯的相对校正因子为1.006 3，RSD（n=5）为0.52%，采用相对校正因子计算的含量与外标法实测值基本一致。结论：一测多评法可用于利胆排石片中木香内酯类成分的含量测定，方法操作简单、省时，结果准确，重复性好，适用于利胆排石片的质量控制。

Objective: To establish a method for determination of costunolide and dehydrocostus lactone in Lidanpaishi tablets by quantitative analysis of multi-components using single marker(QAMS) ,so as to improve the quality.Methods: UPLC was performed on an Acquity UPLC BEH C₁₈ column (2.1 mm×50 mm,1.7 μm) with the mobile phase consisted of methanol-water(50∶50),the flow rate was 0.3 mL·min^-1,the column temperature was 40 ℃,and the detection wavelength was set at 225 nm.Taking costunolide as reference,a relative correction factor(RCF) of dehydrocostus lactone was established.Then the RCF was used to calculate the contents of the dehydrocostus lacton.In this way,the calculated value was compared with the external standard method.Results: The linear ranges of costunolide and dehydrocostus lactone were 0.028-0.42 μg(r=0.999 9) and 0.014-0.21 μg(r=0.999 9),the precision RSD was 1.0% and 0.63%,the repeatability RSD was 1.0% and 1.4%,and the average recoveries(n=6) were 100.5%(RSD=1.6%) and 99.5%(RSD=2.5%).Relative correction factors of dehydrocostus lactone with reference to costunolide were 1.006 3,and the RSD(n=5) was 0.52%.No significant differences were found in the quantitative of dehydrocostus lacton between external standard method and QAMS method.Conclusion: The QAMS method is simple and reliable with a good reproducibility,which is suitable for the analysis and quality control of costuslactone of Lidanpaishi tablets.