左归丸质量标准的研究和探讨

目的：对左归丸的质量标准进行增修提高。方法：增加左归丸中的山药、熟地黄、枸杞子和菟丝子等药材的显微鉴别方法；建立左归丸中熟地黄和枸杞子的薄层色谱鉴别的方法；建立HPLC法测定左归丸中莫诺苷和马钱苷的含量，使用ZORBAX SB-C₁₈ （250 mm×4.6 mm，5 μm）色谱柱，柱温35℃，以乙腈-0.3%磷酸水溶液为流动相，梯度洗脱，流速1.0 mL·min^-1，检测波长240 nm。结果：显微鉴别专属性强，操作简单效果佳；薄层色谱中特征斑点明显，分离度好；莫诺苷和马钱苷进样量分别在0.08~0.80 μg和0.08~0.85 μg范围内线性关系良好，平均回收率分别为101.4%和98.9%，RSD分别为0.60%和2.0%。17批样品中莫诺苷和马钱苷含量范围分别为0.231~0.632 mg·g^-1和0.345~0.604 mg·g^-1，两者含量总和为0.636~1.236 mg·g^-1。结论：本文方法可对左归丸进行准确地定性和定量测定，能够有效评价与控制左归丸质量。

Objective: To revise and improve the quality standard of Zuogui pills.Methods: The microscopic identification methods for Rhizoma Dioscoreae,Rehmanniae Radix Praeparata,Lycii Fructus and Semen Cuscutae in Zuogui pills were established.The TLC methods for the identification of Rehmanniae Radix Praeparata and Lycii Fructus in Zuogui pills were established.HPLC was adopted to determine the content of morroniside and loganin in Zuogui pills.The ZORBAX SB-C₁₈ column(250 mm×4.6 mm,5 μm) was used as the analytical column,the mobile phase was acetonitrile-0.3% phosphoric acid at a flow rate of 1 mL·min^-1 in gradient elution.The column temperature was 25℃ and the detection wavelength was 240 nm.Results: The microscopic identification methods could be performed simply with good specificity.The TLC showed the spots were clear and the separation was good.The calibration curves were linear in the ranges of 0.08-0.80 μg and 0.08-0.85 μg for morroniside and loganin respectively.The mean recoveries of morroniside and loganin were 101.4% and 98.9% with RSDs of 0.60% and 2.0%.For the 17 batches of samples,the amounts of morroniside and loganin were 0.231-0.632 mg·g^-1 and 0.345-0.604 mg·g^-1,and the sum of the two was 0.635-1.236 mg·g^-1.Conclusion: The simple and accurate methods for qualitative and quantitative detection of Zuogui pills can be used in the evaluation and control of the quality of Zuogui pills.