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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,1.7μm),流动相为甲醇-水(50∶50),流速0.3 m L·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0.028~0.42μg(r=0.999 9)和0.014~0.21μg(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 multi-evaluation method for the determination of the content of linalool and dehydrocostus lactone in Lixia Pai tablet. Methods: The mobile phase was methanol-water (50:50) at a flow rate of 0.3 m L · min -1 using the UPLC method on an Acquity UPLC BEH C18 column (2.1 mm × 50 mm, 1.7 μm) 40 ℃, the detection wavelength was 225 nm. The relative calibration factor of debitol was established by using the allyl alcohol as the internal standard, and the relative calibration factors were determined by UPLC method. Lactone content, a measured multiple evaluation of the calculated value and external standard measured values were compared. Results: The linear ranges of the freunds lignocelluloses were 0.028-0.42μg (r = 0.999 9) and 0.014-0.21μg (r = 0.999 9) respectively. The RSDs were 1.0% and 0.63%, respectively. (RSD = 1.6%) and 99.5% (RSD = 2.5%), respectively. The average RSD was 1.0% and 1.4%, respectively. The relative calibration factor of dehydrovaroneol was 1.006 3 and RSD (n = 5) was 0.52%. The content calculated by relative calibration factor was basically the same as that of external standard method. Conclusion: The method of multiple evaluation can be used to determine the content of luxin in Lixia Pai tablet. The method is simple, time-saving, accurate and reproducible. It is suitable for quality control of Lixi Pai Pai tablet.