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两面针质量控制方法改进

Quality control method improvement of Zanthoxylum nitidum

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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GF254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,5 μm);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(R2=1.000 0),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 GF254 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,5 μm),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(R2=1.000 0),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.

Zanthoxylum nitidum(Roxb.)DC.qualitative identificationfingerprintscontent determinationTLCHPLC

安定邦、林启焰、赵祥、程雪梅、王长虹

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上海中医药大学中药研究所,上海中药标准化研究中心,中药标准化教育部重点实验室,上海市复方中药重点实验室,上海 201203

皖西学院生物与制药工程学院,安徽 六安 237012

两面针 定性鉴别 指纹图谱 含量测定 TLC HPLC

国家药典委员会药品标准制修订任务项目上海市卫生健康委中医药传承创新发展三年行动计划建设项目

2018Z0122018-2020-CCCX-5002

2024

中成药
国家食品药品监督管理局,信息中心中成药信息站,上海中药行业协会

中成药

CSTPCD北大核心
影响因子:1.217
ISSN:1001-1528
年,卷(期):2024.46(5)
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