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目的:研究紫草渗漉液浓缩过程中左旋紫草素的损失原因并建立合理检测方法。方法:以左旋紫草素为指标,采用优化的色谱条件进行测定,分析检测环节中供试液含醇量、供试液生药浓度等对左旋紫草素含量测定的影响,在此基础上考察供试液合理制备方法及含量测定方法学,以建立合理的检测方法。结果:优化的色谱条件为:甲醇∶水(82∶18)为流动相,流速:1.0 mL/min,柱温为35℃,检测波长为516 nm,将分析时间由40 min缩短为24 min;供试液的含醇量显著影响左旋紫草素的含量测定结果,同等浓度的左旋紫草素,在低含醇量(<40%)供试液中的峰面积仅约为高含醇量(>70%)的20%～30%;供试液最好用40%以上乙醇配制,合理浓度范围为0.0167～0.083 g生药/mL;改进的检测方法具有良好的精密度、重现性和准确性。结论:研究首次发现供试液含醇量与左旋紫草素的色谱峰面积密切相关,并由此揭示紫草渗漉液回收乙醇过程中“巨大损失”的另一重要原因是:在检测环节中,供试液含醇量过低导致左旋紫草素的测定结果显著偏低,未能客观反映实际含量。新方法较现有方法能更有效、合理、客观的检测左旋紫草素,监测工艺过程,同时具有高效率、低成本的优势。
OBJECTIVE: To study the cause of L-shikonin loss in the process of concentration of comfrey percolate and to establish a reasonable detection method. Methods: Taking shuanghuangshuang as an index, the optimal chromatographic conditions were used for the determination. The influence of alcohol content in the test solution and the crude drug concentration of the test solution on the determination of L-shikonin was analyzed. On the basis of this, For the test solution reasonable preparation methods and content determination methodologies to establish a reasonable detection method. Results: The optimized chromatographic conditions were as follows: methanol: water (82:18) as mobile phase, the flow rate was 1.0 mL / min, the column temperature was 35 ℃, the detection wavelength was 516 nm and the analysis time was shortened from 40 min to 24 min. The alcohol content of the test solution significantly affect the determination of levosulfate content, the same concentration of levosirin, low alcohol content (<40%) for the test solution peak area is only about high alcohol content (> 70%) of 20% ~ 30%; the best test solution prepared with more than 40% ethanol, a reasonable concentration range of 0.0167 ~ 0.083 g crude drug / mL; improved detection method with good precision, reproducibility and accuracy. Conclusion: The first study found that the alcohol content of the test solution is closely related to the chromatographic peak area of L-shikonin, and thus another important reason for the “huge loss” in the process of ethanol recovery from shikoki percolate is that at In the testing process, the low alcohol content of the test solution resulted in a significantly lower measurement result of L-shikonin, which failed to objectively reflect the actual content. Compared with the existing methods, the new method can detect L-shikonin more effectively, reasonably and objectively, and can monitor the technological process with advantages of high efficiency and low cost.