蒙药复方制剂孟根·沃斯-18丸质量标准研究

Study on Quality Standard of Mongolian Medicine Compound Preparation Mengen Vos-18 Pills

目的建立蒙药复方制剂孟根·沃斯-18丸质量标准。方法对制剂进行显微鉴别,采用薄层色谱(TLC)法定性鉴别制剂中枫香脂;采用滴定法测定热制水银的含量;采用高效液相色谱法测定6种生物碱含量,色谱柱为Agilent Eclipse Plus C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-0.2%磷酸水溶液(梯度洗脱),流速为1.0 mL/min,检测波长为232 nm,柱温为40℃,进样量为10μL。结果制剂显微鉴别特征明显;枫香脂的TLC图斑点清晰,分离度好,阴性对照无干扰;热制水银重复性试验结果的RSD为1.63%,平均加样回收率为100.50%(RSD=1.99%,n=9);苯甲酰新乌头原碱、苯甲酰次乌头原碱、苯甲酰乌头原碱、新乌头碱、次乌头碱、乌头碱进样量分别在45.19~293.72μg、4.73~30.73μg、6.33~41.17μg、9.28~60.33μg、8.78~57.09μg、9.31~60.52μg范围内与峰面积线性关系良好(r=0.9999),精密度、稳定性、重复性试验结果的RSD均小于3.0%,平均加样回收率分别为93.24%,95.68%,92.13%,89.59%,88.30%,89.82%,RSD分别为2.34%,2.45%,3.13%,2.61%,2.69%,3.22%(n=9)。10批次制剂中热制水银含量为9.42%~13.83%,转移率为96.97%;单酯型生物碱(苯甲酰新乌头原碱、苯甲酰次乌头原碱、苯甲酰乌头原碱)总量为7.7~62.0μg/g、双酯型生物碱(新乌头碱、次乌头碱、乌头碱)总量为9.0~49.0μg/g。结论所建方法操作简便,专属性强,可为含草乌中蒙药制剂标准的建立提供参考。

Objective To establish the quality standard of the Mongolian medicine compound preparation Mengen Vos-18 Pills.Methods The microscopic identification was performed on the preparation,and the thin-layer chromatography(TLC)method was used to qualitatively identify Liquidambaris Resina in the preparation.The titration method was used to determine the thermal mercury.The high-performance liquid chromatography(HPLC)method was used to determine six alkaloids;the chromatographic column was the Agilent Eclipse Plus C18 column(250 mm×4.6 mm,5μm),the mobile phase was acetonitrile-0.2%phosphoric acid aqueous solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelength was 232 nm,the column temperature was 40℃,and the injection volume was 10μL.Results The microscopic identification characteristics of the preparation were obvious.The TLC chromatogram of Liquidambaris Resina showed clear spots,good resolution,with no interference from the negative reference.The RSDs of the repeatability test for thermal mercury was 1.63%,and its average recovery rate was 100.50%with an RSD of 1.99%(n=9).The linear ranges of benzoylmesaconine,benzoylhypaconine,benzoylaconine,mesaconitine,hypaconitine,and aconitine were 45.19-293.72μg,4.73-30.73μg,6.33-41.17μg,9.28-60.33μg,8.78-57.09μg,9.31-60.52μg(r=0.9999)respectively;the RSDs of precision,stability and repeatability tests were all lower than 3.0%;the average recovery rates of the above six components were 93.24%,95.68%,92.13%,89.59%,88.30%,89.82%,with the RSDs of 2.34%,2.45%,3.13%,2.61%,2.69%,3.22%(n=9),respectively.The thermal mercury content in the 10 batches of preparations was in the range of 9.42%-13.83%,with a transfer rate of 96.97%.The total amount of monoester-alkaloids(benzoylmesaconine,benzoylhypaconine,benzoylaconine)was in the range of 7.7-62.0μg/g,and the total amount of diester-alkaloids(mesaconitine,hypaconitine,aconitine)was in the range of 9.0-49.0μg/g.Conclusion The established method is easy and specific,which can provide a reference for the establishment of standards for Chinese and Mongolian medicine preparations containing Aconiti Kusnezoffii Radix.