| 引用本文: | 周智文,刘豪,朱纲,姚建标,周鑫,王建方,王如伟.基于一测多评法鉴别蓝芩制剂中的黄柏与关黄柏[J].中国现代应用药学,2023,40(10):1360-1366. |
| ZHOU Zhiwen,LIU Hao,ZHU Gang,YAO Jianbiao,ZHOU Xin,WANG Jianfang,WANG Ruwei.Identification of Phellodendri Chinensis Cortex and Phellodendri Amurensis Cortex in Lanqin Preparation by QAMS[J].Chin J Mod Appl Pharm(中国现代应用药学),2023,40(10):1360-1366. |
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| 基于一测多评法鉴别蓝芩制剂中的黄柏与关黄柏 |
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周智文1, 刘豪2,3, 朱纲2,3, 姚建标2,3, 周鑫2,3, 王建方2,3, 王如伟1
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1.浙江中医药大学药学院, 杭州 310053;2.浙江康恩贝制药股份有限公司, 杭州 310052;3.浙江省中药制药技术重点实验室, 杭州 310052
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| 摘要: |
| 目的 建立蓝芩制剂中盐酸黄柏碱、盐酸巴马汀及盐酸小檗碱的HPLC一测多评法,并基于含量测定结果建立蓝芩制剂中黄柏与关黄柏的鉴别方法。方法 采用Agilent 1260色谱仪,Waters Atlantis T3(250 mm×4.6 mm,5 μm)色谱柱,以乙腈-0.2%磷酸溶液(每100 mL加十二烷基磺酸钠0.2 g)梯度洗脱,流速为1 mL·min-1,检测波长为280 nm,柱温30℃,以盐酸小檗碱为参照物,计算盐酸黄柏碱及盐酸巴马汀的相对校正因子,所得结果与外标法结果进行比较,判断该方法的可靠性。利用聚类分析含量测定结果,讨论黄柏与关黄柏对3种生物碱含量的影响,建立鉴别方法,对不同厂家的蓝芩制剂进行测定。结果 盐酸黄柏碱、盐酸巴马汀及盐酸小檗碱分别在1.087~54.35 μg·mL-1,0.100 9~20.18 μg·mL-1,0.536 5~26.82 μg·mL-1内线性关系良好;平均加样回收率分别为91.57%(RSD=3.0%),97.96%(RSD=2.1%),100.6%(RSD=1.1%);相对校正因子分别为0.368,1.239。所得结果与外标法所测结果的RSD<2%,2种方法无显著差异。聚类分析显示使用黄柏与使用关黄柏的蓝芩制剂3种生物碱含量有明显差异;以盐酸黄柏碱与盐酸巴马汀的含量比值为鉴别标准,建议蓝芩制剂中"盐酸黄柏碱与盐酸巴马汀含量比值不得<2.5",不同厂家的蓝芩制剂测定结果均符合标准,表明工艺与原料对本方法无显著影响。结论 本研究建立了蓝芩制剂的HPLC一测多评法,并建立了蓝芩制剂中黄柏与关黄柏的鉴别方法,方法可信度高,为蓝芩制剂的质量提升提供了参考。 |
| 关键词: 一测多评法 蓝芩制剂 鉴别 黄柏 关黄柏 |
| DOI：10.13748/j.cnki.issn1007-7693.20221397 |
| 分类号:R917 |
| 基金项目:国家药品监督管理局中成药质量评价重点实验室开放课题(GZYZZ2020002) |
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| Identification of Phellodendri Chinensis Cortex and Phellodendri Amurensis Cortex in Lanqin Preparation by QAMS |
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ZHOU Zhiwen1, LIU Hao2,3, ZHU Gang2,3, YAO Jianbiao2,3, ZHOU Xin2,3, WANG Jianfang2,3, WANG Ruwei1
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1.School of Pharmaceutical Sciences, Zhejiang Chinese Medical University, Hangzhou 310053, China;2.Zhejiang CONBA Pharmaceutical Co., Ltd., Hangzhou 310052, China;3.Zhejiang Provincial Key Laboratory of Traditional Chinese Medicine Pharmaceutical Technology, Hangzhou 310052, China
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| Abstract: |
| OBJECTIVE To establish an HPLC qualitative analysis of multi-components by single-marker(QAMS) method for the determination of phellodendron hydrochloride, palmatine hydrochloride and berberine hydrochloride in Lanqin preparation, and to establish a method for the identification of Phellodendri Chinensis Cortex and Phellodendri Amurensis Cortex in Lanqin preparation based on the content determination results. METHODS Using Agilent 1260 chromatograph and Waters Atlantis T3 column(250 mm×4.6 mm, 5 μm), the chromatographic column was gradient eluted with acetonitrile-0.2% phosphoric acid solution(0.2 g sodium dodecyl sulfonate per 100 mL), the flow rate was 1 mL·min-1, the detection wavelength was 280 nm, the column temperature was 30℃, and the relative correction factors of phellodendron hydrochloride and palmatine hydrochloride were calculated with berberine hydrochloride as the reference. The results were compared with the results of external standard method to judge the reliability of the method. Based on the results of cluster analysis, the effects of Phellodendri Chinensis Cortex and Phellodendri Amurensis Cortex on the contents of three alkaloids were discussed, and the identification method was established to determine the Lanqin preparations from different manufacturers. RESULTS The concentrations of phellodendron hydrochloride, palmatine hydrochloride and berberine hydrochloride had good linear relationship within 1.087-54.35 μg·mL-1, 0.100 9-20.18 μg·mL-1 and 0.536 5-26.82 μg·mL-1 respectively. The average recoveries were 91.57%(RSD=3.0%), 97.96%(RSD=2.1%) and 100.6%(RSD=1.1%). The relative correction factors were 0.368 and 1.239, respectively. The RSD between the obtained results and the results measured by the external standard method was < 2%, and there was no significant difference between the two methods. Cluster analysis showed that there were significant differences in the contents of three alkaloids between Lanqin granule and its adulterants. Taking the content ratio of phellodine hydrochloride to palmatine hydrochloride as the identification standard, it was suggested that "the content ratio of phellodine hydrochloride to palmatine hydrochloride should not be < 2.5" in Lanqin preparation. The determination results of Lanqin preparation from different manufacturers were in line with the standard, indicated that the process and raw materials have no significant impact on this method. CONCLUSION In this study, an HPLC-QAMS for Lanqin preparation, and the identification method of Phellodendri Chinensis Cortex and Phellodendri Amurensis Cortex in Lanqin preparation is established, which with high reliability of the method provided a reference for the quality improvement of Lanqin preparation. |
| Key words: QAMS Lanqin preparation identify Phellodendri Chinensis Cortex Phellodendri Amurensis Cortex |
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