降脂方中活性成分含量测定方法

Determination Method of Active Ingredients in Jiangzhi Prescription(降脂方)

目的:建立降脂方中蒽醌类成分和总生物碱的含量测定方法。方法:采用HPLC法,Agilent Eclipse XDB-C18色谱柱(4.6 mm×250 mm,5μm),以乙腈-0.1%磷酸溶液(40∶60)为流动相,流速为1 mL/min,检测波长为284 nm,柱温为40℃,同时测定橙黄决明素、黄决明素、决明素、决明蒽醌4种蒽醌类成分;以荷叶碱为对照品,采用酸性染料比色法测定降脂方总生物碱的含量。结果:4种蒽醌类成分分别在各自检测范围内呈良好的线性关系(r>0.999 9);精密度、稳定性、重复性试验的RSD<2%;加样回收率分别为98.36%~102.45%、97.56%~102.83%、99.47%~103.39%、100.08%~104.25%,RSD分别为1.68%、2.07%、1.60%、1.76%(n=6)。荷叶碱在30.72~107.52μg范围内与吸光度有良好的线性关系,线性回归方程Y=0.006 8X-0.014 4,r=0.999 8,平均回收率102.10%,RSD为1.91%。结论:该方法具有一定的专属性和准确度,灵敏度高,简便易行。

Objective: To establish a method for the determination anthraquinones and total alkaloids in Jiangzhi Prescription. Methods: Agilent Eclipse XDB-C18 chromatographic column(4.6 mm ×250 mm, 5 μm) was used, with acetonitrile-0.1% phosphoric acid solution(40:60) as the mobile phase, the flow rate was 1 mL/min,the detection wavelength was 284 nm, and the column temperature was 40 ℃. This chromatographic method was used to simultaneously determine the four anthraquinone components of aurantio-obtusin, chrysoobtusin, obtusin,and obtusifolin. With nuciferine as the reference substance, the total alkaloid content of Jiangzhi Prescription was determined by the acid dye colorimetric method. Results: The four anthraquinone components showed a good linear relationship within their respective detection ranges(r>0.999 9). The RSD of the precision, stability, and repeatability tests were lower than 2%. The sample recovery rates were 98.36%-102.45%, 97.56%-102.83%,99.47%-103.39%, 100.08%-104.25%, and the RSD were 1.68%, 2.07%, 1.60%, 1.76%(n=6). Nuciferine had a good linear relationship with absorbance in the range of 30.72-107.52 μg. The linear regression equation was Y=0.006 8X-0.014 4, r=0.999 8. The average recovery rate was 102.10%, and the RSD was 1.91%. Conclusion: The method has certain specificity and accuracy, high sensitivity, simple and easy to implement.