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目的:建立HPLC法同时测定钩吻茎中胡蔓藤碱丙、钩吻素甲、钩吻素子、钩吻素己、钩吻绿碱和胡蔓藤碱乙的含量,并比较评价各产地钩吻生物碱含量的差异。方法:采用外标法进行测定,色谱柱为ZORBAX Bonus-RP Analytical(4.6 mm×250 mm,5μm),流动相为甲醇-0.1%甲酸水梯度洗脱,流速1.0 m L·min~(-1),检测波长254 nm,柱温30℃。分别测定32批钩吻茎,并进行聚类分析。结果:胡蔓藤碱丙、钩吻素甲、钩吻素子、钩吻素己、钩吻绿碱、胡蔓藤碱乙6个成分的线性范围分别为1.00~50.06μg·mL~(-1)(r=1.000 0)、1.13~50.85μg·mL~(-1)(r=0.999 8)、1.16~52.20μg·mL~(-1)(r=1.000 0)、1.16~52.20μg·mL~(-1)(r=0.999 7)、1.06~50.88μg·mL~(-1)(r=0.999 7)和1.01~50.50μg·mL~(-1)(r=1.000 0),平均加样回收率为93.1%~103.8%(RSD为2.0%~2.9%)。不同产地样品中钩吻茎中胡蔓藤碱丙、钩吻素甲、钩吻素子、钩吻素己、钩吻绿碱和胡蔓藤碱乙含量范围分别为0.136~2.202、0.564~2.686、0.718~3.553、0.160~2.025、0.151~3.493、0.288~4.700 mg·g~(-1)。结果显示不同产地的钩吻6个成分含量均有差异,32批不同产地钩吻药材可聚为6大类。结论:该法可为钩吻多指标成分的质量评价提供参考。不同产地钩吻的各个化学成分的含量呈现明显分类特点,为钩吻地区鉴定提供依据。
OBJECTIVE: To establish a HPLC method for the simultaneous determination of ursinae, caenorubicin, capecitabine, capecitabine, cauliflower, and vinesine B in the experimental group, and to compare the contents of causal alkaloids The difference. Methods: The external standard method was used for the determination. The mobile phase consisted of gradient elution with methanol-0.1% formic acid and the mobile phase was 1.0 mL · min -1 ), Detection wavelength 254 nm, column temperature 30 ℃. 32 batches of hook-and-shoot hooks were determined and clustered. Results: The linear range of the contents of the four components, vincristine, cinchon, crookolin, crocin, gallic acid, ethamemine B were 1.00-50.06 μg · mL -1 (r = 1.16 ~ 52.20μg · mL -1 (r = 1.000 0), 1.16 ~ 52.20μg · mL -1 (r = 0.999 8), 1.13 ~ 50.85μg · mL -1 (r = 0.999 7), 1.06-50.88μg · mL -1 (r = 0.999 7) and 1.01-50.50μg · mL -1 (r = 1.000 0) respectively. The average recoveries were 93.1% ~ 103.8% (RSD 2.0% -2.9%). In different samples from different areas, the content of albumin, acenaphthene, kylogenin, piriformin, gachydine and ethamectin in the samples from different areas were 0.136 ~ 2.202, 0.564 ~ 2.686 and 0.718 ~ 3.553, 0.160 ~ 2.025,0.151 ~ 3.493,0.288 ~ 4.700 mg · g ~ (-1). The results showed that the content of 6 components of kyphus kiss in different areas were different, and 32 batches of kamika drug in different areas could be grouped into 6 categories. Conclusion: This method can provide reference for the quality evaluation of multiple index components of hook kisses. The content of each chemical composition of kissing in different areas showed obvious classification features, which provided the basis for the identification of the kissing area.