中国药典中桑叶含量测定项下色谱条件的优化

目的： 优化中国药典中桑叶含量测定项下的色谱条件。 方法： 采用LC-MS联用技术和标准加入法鉴定中国药典方法下"芦丁"峰的纯度；优化后的色谱条件：Diamonsil^TM C₁₈（250 mm×4.6 mm，5 μm），以乙腈（A）-0.2%甲酸水溶液（B）为流动相，梯度洗脱（0 min，18%A；0～5 min，18%A→20%A；5～7 min，20%A→22%A；7～24 min，22%A→23%A），流速0.8 mL·min^-1，检测波长358 nm，柱温30℃，进样量10 μL。 结果： 2010年版中国药典（一部）桑叶的含量测定项下"芦丁"峰实际是芦丁与异槲皮苷的混合峰；优化后的方法实现了芦丁和异槲皮苷的基线分离，其线性范围分别为0.222～8.88 μg（r=0.9999）、0.143～5.72 μg（r=0.9999）；平均回收率（n=5）分别为100.8%（RSD=1.6%）、100.5%（RSD=1.4%）。 结论： 优化后的方法简便，重复性好，可以客观准确地用于桑叶药材的质量控制，为中国药典中桑叶质量标准的修订提供科学依据。

Objective: To optimize the chromatographic conditions in the determination method of Mori Folium(mulberry leaf)in Chinese Pharmacopoeia. Methods: The purity of "rutin" was identified by combined use of the pharmacopeia LC-MS method and adding standards.The analyses were performed on Diamonsil^TM C₁₈ columns (250 mm×4.6 mm,5 μm)with the gradient elution (0 min,18%A;0-5 min,18%A→20%A;5-7 min,20%A→22%A;7-24 min,22%A→23%A)of acetonitrile(A)-0.2% formic acid(B)aqueous at a flow rate of 0.8 mL·min^-1.The detection wavelength was set at 358 nm and the column temperature was controlled at 30℃.The injection volume was 10 μL. Results: The peak of rutin obtained from the pharmacopeial method was actually mixed with rutin and isoquercitrin.Rutin and isoquercitrin were separated successfully using the optimized method,and good linearity was obtained for the two contents in the ranges of 0.222-8.88 μg(r=0.9999)and 0.143-5.72 μg(r=0.9999),respectively.The average recoveries(n=5)of the two constitutions were 100.8%(RSD=1.6%)and 100.5%(RSD=1.4%)respectively. Conclusion: The optimized method,which is simple and reproducible,can be used for the quality control of Mori Folium.This study provides a scientific basis for the revise of the quality standards of Mori Folium in Chinese Pharmacopoeia.

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