两面针质量控制方法改进

Quality control method improvement of Zanthoxylum nitidum

目的改进两面针质量控制方法。方法在氯化两面针碱、白屈菜红碱、毛两面针素的TLC定性鉴别中,分析采用硅胶GF_(254)薄层板,以氯仿-甲醇-氨水(30∶1∶0.1)为展开剂。建立两面针及其混淆品HPLC指纹图谱。在木兰花碱、氯化两面针碱、白屈菜红碱的HPLC含量测定中,分析采用Diamonsil Plus色谱柱(250 mm×4.6 mm,5μm);流动相乙腈-0.1%三氟乙酸,梯度洗脱;体积流量1.0 mL/min;柱温30℃;检测波长273 nm。结果TLC斑点清晰,分离度良好。18批药材指纹图谱相似度为0.484~0.983,两面针及其混淆品得到有效区分。3种成分在各自范围线性关系良好(R^(2)=1.0000),平均加样回收率98.9%~103.3%,RSD 1.17%~1.96%。结论该方法简便,重复性好,可为两面针质量控制提供一种新方法。

AIM To improve the quality control method of Zanthoxylum nitidum(Roxb.)DC.METHODS In the TLC qualitative identification of nitidine chloride,chelerythrine and toddalolactone,the analysis was performed on silica gel GF_(254)TLC plate,chloroform-methanol-ammonia(30∶1∶0.1)was taken as a developing agent.The HPLC fingerprints for Z.nitidum and its adulterants were established.In the HPLC content determination of magnoflorine,nitidine chloride and chelythrine,the analysis was performed on a 30℃thermostatic Diamonsil Plus column(250 mm×4.6 mm,5μm),with the mobile phase comprising of acetonitrile-0.1%trifluoroacetic acid flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelength was set at 273 nm.RESULTS The clear TLC plots demonstrated good separation.The similarities of fingerprints for eighteen batches of medicinal materials were 0.484-0.983,Z.nitidum and its adulterants were effectively distinguished.Three constituents showed good linear relationships within their own ranges(R^(2)=1.0000),whose average recoveries were 98.9%-103.3%with the RSDs of 1.17%-1.96%.CONCLUSION This simple and reproducible can provide a new method for the quality control of Z.nitidum.