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夏杰,贾巧君,叶子弘,杨东风,侯卓妮,肖艺,张晓丹.丹参新酮标准样品的研制[J].湖南中医药大学学报英文版,2021,41(11):1711-1716.[Click to copy
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| 丹参新酮标准样品的研制 |
| 夏杰,贾巧君,叶子弘,杨东风,侯卓妮,肖艺,张晓丹 |
| (浙江理工大学生命科学与医药学院, 浙江 杭州 310012;浙江理工大学生命科学与医药学院, 浙江 杭州 310012;浙江省植物次生代谢调控重点实验室, 浙江 杭州 310012;中国计量大学生命科学学院, 浙江 杭州 310012;浙江省宁波易中禾药用植物研究院有限公司, 浙江 宁波 315000) |
| 摘要: |
| 目的 根据GB/T15000.3-2008《标准样品工作导则（3）标准样品：定值的一般原则和统计方法》和GB/T15000.5-2008《标准样品工作导则（5）标准样品：化学成分标准样品技术通则》中指导要求，在国家标准化技术管理委员会批准立项的基础上，开展关于丹参新酮标准样品的研制。方法 以唇形科鼠尾草属药用植物陕南道地丹参（Salvia miltiorrhiza Bge）为原料通过醇提、硅胶柱色谱分离、制备色谱得到丹参新酮纯品；采用红外分光光度分析法（IR）、紫外光谱（UV）、核磁共振（NMR）和质谱（MS）等波谱技术对其进行定性分析和结构确证。将样品分装成100瓶（10 mg/瓶），采用高效液相色谱法（HPLC）进行均匀性和稳定性检验以及联合定值分析。结果 经检验该样品在95%的置信区间范围内均匀性良好；在0~4℃的条件下，24个月内稳定性良好；采用多个实验室协作试验定值，丹参新酮标准样品的纯度为99.350%，扩展不确定度0.053%。结论 丹参新酮达到国家标准样品的技术要求，丹参新酮标准样品批号GSB 11-3803-2020可以用于丹参药材及其副产品中丹参新酮含量的测定、结构的确定、质量甄别、检测方法的校正和质量控制，为药材和产品成分检测结果的准确性、对比性、可溯性提供参考。 |
| 关键词: 丹参新酮 标准样品 均匀性 稳定性 定值 不确定度 |
| DOI：10.3969/j.issn.1674-070X.2021.11.011 |
| Received:May 01, 2021 |
| 基金项目:中央本级重大增减支项目（2060302）；2019年度宁波市“泛3315”创业团队计划（现代农业领域C类创业团队）。 |
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| Preparation of Miltirone Standard Sample |
| XIA Jie,JIA Qiaojun,YE Zihong,YANG Dongfeng,HOU Zhuoni,XIAO Yi,ZHANG Xiaodan |
| (College of Life Sciences and Medicine, Zhejiang Sci-Tech University, Hangzhou, Zhejiang 310012, China;College of Life Sciences and Medicine, Zhejiang Sci-Tech University, Hangzhou, Zhejiang 310012, China;Laboratory of Plant Secondary Metabolism and Regulation of Zhejiang Province, Hangzhou, Zhejiang 310012, China;College of Life Sciences, China Jiliang University, Hangzhou, Zhejiang 310012, China;Yizhonghe Medicinal Plants Research Institute of Zhejiang Ningbo, Ningbo, Zhejiang 315000, China) |
| Abstract: |
| Objective According to the guiding requirements of GB/T15000.3-2008 Guidelines for Standard Samples (3):General Principles and Statistical Methods of Fixed Value and GB/T15000.5-2008 Guidelines for Standard Samples (5):Technical General Rules of Chemical Composition Standard Samples, on the basis of the approval of the project by the National Standardization Technical Management Committee, the standard sample of miltirone was developed. Methods Salvia miltiorrhiza Bge, a medicinal plant of Salvia of Labiatae, was used as raw material. The pure miltirone was obtained by alcohol extraction, silica gel column chromatography, preparative chromatography respectively. Infrared spectrophotometry (IR), ultraviolet spectroscopy (UV), nuclear magnetic resonance (NMR) and mass spectrometry (MS) were used for qualitative analysis and structural confirmation. The samples were divided into 100 bottles (10 mg/bottle), and then the uniformity and stability were tested by high performance liquid chromatography (HPLC) method, and the combined fixed value analysis was carried out. Results The results of the study indicated that the sample had good uniformity within 95% confidence interval. It was stable within 24 months at 0~4℃. Multiple laboratories were used to cooperate to test the setting value, the purity of standard sample of miltirone was 99.35% and the expanded uncertainty was 0.053%. Conclusion Miltirone meets the technical requirements of national standard samples, and the standard sample batch number GSB 11-3803-2020 can be used for the determination of the content of salvia miltiorrhiza Bge and its by-products, the determination of the structure, the quality screening, the calibration and quality control of the detection method, and provide reference for the accuracy, comparability and traceability of the detection results of the medicinal materials and the product components. |
| Key words: miltirone standard sample uniformity stability constant value uncertaint |
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