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目的:采用特征图谱法对不同产地的蟾皮药材进行了分析,并建立了同时测定沙蟾毒精等4种蟾毒配基类成分的含量的方法,为其质量控制和药材鉴定提供依据。方法:采用特征图谱法对不同产地的多批蟾皮药材进行了沙蟾毒精等4种蟾毒配基类成分的含量测定。采用菲罗门Phenomenex Gemini色谱柱(4.6 mm×250 mm,5μm),流动相乙腈(A)-水(B)梯度洗脱(0~30 min,10%~45%A;30~45 min,45%~60%A),流速1.0 m L·min-1,柱温35℃,检测波长296 nm。结果:四川产地蟾皮的沙蟾毒精含量较高(大花皮、中黑皮、超大皮、棕褐色皮、小黑皮质量分数分别是0.252 4%,0.158 4%,0.181 1%,0.125 8%,0.108 8%),其次是江苏产地的黑皮(0.227 5%)。四川大花皮中华蟾毒它灵含量较高(0.214 3%),其次是江苏黑皮(0.147 8%)。四川小黑皮中蟾毒灵(0.051 0%)和山东小花皮中华蟾酥毒基(0.136 1%)含量较其他产地和品种中较高。总体来说,四川产地的蟾皮4种配基类含量较高,尤其是四川大花皮品种。结论:该文采用特征图谱法对不同产地蟾皮中沙蟾毒精进行了测定,并对其他3种蟾毒配基类成分进行了标定,该方法准确可靠,可用于蟾皮的鉴别和质量控制。不同产地和品种蟾皮中4种蟾毒配基类成分含量不尽相同。
OBJECTIVE: To analyze the contents of toad skin medicinal materials in different areas by the method of feature mapping, and to establish a method for the simultaneous determination of four kinds of bufalin and other bufalodine ligand components for their quality control and medicinal materials identification. Methods: The contents of 4 kinds of bufalin ligands of safin bufogenin were determined by the method of characteristic map. The mobile phase was eluted with Phenomenex Gemini column (4.6 mm × 250 mm, 5 μm) and mobile phase of acetonitrile-water (B) gradient (0-30 min, 10% -45% A, 30-45 min, 45% -60% A) at a flow rate of 1.0 m L · min-1. The column temperature was 35 ℃ and the detection wavelength was 296 nm. Results: The content of safrole in the toad skin of Sichuan origin was high (mass fraction of big flower, middle black, large skin, tan skin and black skin were 0.252 4%, 0.158 4%, 0.181 1%, 0.125 8%, 0.108 8%), followed by black skins originating in Jiangsu (0.227 5%). Sichuan Huahuabu caffetum its spirit content is high (0.214 3%), followed by Jiangsu black skin (0.147 8%). The content of bufalin (0.051 0%) in Sichuan black skin and the Chinese cinobufagin (0.136 1%) in Shandong small flower skin were higher than those in other areas. In general, the contents of four kinds of ligands in the toad skin of Sichuan origin are relatively high, especially in Sichuan. Conclusion: The method of eigen-fingerprinting was used for the determination of resibufogenin in toad skin from different areas. The calibration of the other three kinds of bufadroxidins was also confirmed. The method is accurate and reliable and can be used for identification and quality of toad skin control. The content of the four kinds of bufadanin in different areas and varieties of toad skin varied with different base components.