摘要
目的：利用HPLC-DAD对不同批次银杏叶片进行分析，建立银杏叶片的质量控制方法。方法：采用AgilentPoroshell 120 SB C_18色谱柱（4．6mm×150mm，2．7μm），流动相甲醇-0．2％磷酸水梯度洗脱，检测波长265nm，流速0．5mL·min-1，柱温35℃。对14批银杏叶片进行分析，建立银杏叶片的指纹图谱，并采用系统指纹定量法进行质量评价，同时测定了芦丁、槲皮素、山奈素和异鼠李素4个成分的含量，用系统聚类法进行分析。结果：根据建立的指纹图谱得出除S6，S7，S8外，其他批次在化学指纹数量与含量分布比例相似度良好（S_m≥0．95），而体现化学指纹整体含量的P_m（42．3～133．2）差异较大。按系统指纹定量法鉴定出14批样品分为7个不同的质量等级，除S1，S6，S8，S9，S10外，其他样品质量等级均在5级以下，质量较好；4个成分的含量测定方法有良好的精密度、重复性、稳定性，测定结果显示14批样品含量差异较大（RSD22．5％），其中S7含量最高，S14含量最低，系统聚类分析分为5类。结论：综合多成分定量测定及化学定量指纹图谱分析方法能较全面地表征不同批次银杏叶片的整体和部分内在成分差异，可为银杏叶片质量控制提供参考。
Objective： To establish the method for identification and quality control of Ginkgo tablet （GT） of different batches by analysis using HPLC-DAD. Method： Agilent Poroshell 120 SB Cls （4.6 mm × 150 mm, 2.7 μm） was used as the separation column. The analyses were performed on condition of gradient elution solvents of methanol and 0. 2% phosphoric acid. The flow rate was 0. 5 mL· min-1, detecting wavelength was 265 nm and column temperature was 35 ℃The fingerprint chromatogram was established and evaluated by systematically quantified fingerprint method （SQFM）. Meanwhile, four components including rutin （RT）, quercetin （QC）, kaempferol （KF） and isorhamnetin （IR） of 14 batches of GT were determined and classified by hierarchical clustering method. Result： According to the established fingerprint, the chemical proportion and concentration distribution is similar with S_m more than 0.95 except for S6, S7 and S8, while great difference existed among the value of P in the range of 42.3 to 133.2. As the SQFM, the 14 batches of sample fell into seven different quality levels. Except for S1, S6, S8, S9 and S10, the other batches were all evaluated as lower than grade 5 which represents a good quality. The method of content determination was desirable precision,reproducibility, and stability. The result showed that the total contents of four components varied greatly （RSD - 22.5% ）. Among the 14 batches of GTs, the total content in S7 was the highest while S14 was reverse. The samples were clustered into five types. Conclusion： Indicates that inner difference of the chemical component in various batches of GT can be reflected by this method, which can be used for quality control.
出处
《中国实验方剂学杂志》
CAS
北大核心
2014年第12期52-57,共6页
Chinese Journal of Experimental Traditional Medical Formulae
基金
国家自然科学基金重大研究计划项目(90612002)
国家基础科学人才培养基金项目(J1103606)
关键词
银杏叶片
定量指纹图谱
系统指纹定量法
Ginkgo tablet
quantified fingerprint
systematically quantified fingerprint method
