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目的:对败酱片(黄花败酱)建立质量标准。方法:以齐墩果酸、熊果酸为对照品,对方中败酱建立TLC鉴别;用高效液相色谱法对方中齐墩果酸、熊果酸进行测定。色谱条件:迪马Kr C18;流动相:乙腈-甲醇-水-乙酸铵(70∶10∶20∶0.5);流速:1.0 mL/min;柱温:30℃;检测波长:215 nm。供试品溶液的制备:取样品约4 g,加入乙醇30 mL,置85℃水浴中加热回流提取,分取乙醇提取液15 mL,蒸干,残渣加盐酸溶液(2→10)10 mL水解1 h,用三氯甲烷液萃取,将萃取液蒸干,残渣加甲醇使溶解并定容,即得。结果:齐墩果酸在0.476 8~9.536 0μg范围内呈线性关系,平均加样回收率为99.5%;熊果酸在0.651 0~13.020 0μg范围内呈线性关系,平均加样回收率为103.3%。结论:本法操作简便,结果准确,重现性好,可以控制败酱片的质量。
Objective: To establish a quality standard for the sauerkraut sauce. METHODS: The oleanolic acid and ursolic acid were used as the reference substance. The TPC was used to establish the identification method of the other sauce. The content of oleanolic acid and ursolic acid were determined by high performance liquid chromatography. Chromatographic conditions: Dima Kr C18; mobile phase: acetonitrile-methanol-water-ammonium acetate (70:10:20:0.5); flow rate: 1.0 mL/min; column temperature: 30°C; detection wavelength: 215 nm. Preparation of the test solution: take about 4 g of the sample, add 30 mL of ethanol, heat and reflux at 85 °C in a water bath, separate and take 15 mL of the ethanol extract, and evaporate to dryness. Add 10 mL of hydrochloric acid solution (2→10) to the residue. After 1 h, the mixture was extracted with chloroform, and the extract was evaporated to dryness. Methanol was added to the residue to dissolve and determine the volume. Results: The content of oleanolic acid was linear in the range of 0.476 8~9.5536 0μg. The average recovery was 99.5%. The content of ursolic acid was linear in the range of 0.651 0~13.020 0μg. The average recovery was 103.3%. . Conclusion: This method is simple, accurate and reproducible. It can control the quality of the sauce.