[1]耿岩玲,王晓,朱姮,等.白鲜皮中黄柏酮标准样品的研制[J].江苏农业学报,2018,(04):933-937.[doi:doi:10.3969/j.issn.1000-4440.2018.04.031]
　GENG Yan-ling,WANG Xiao,ZHU Heng,et al.Preparation of certified reference materials of obacunone from bark of Dictamnus dasycarpus Turcz[J].,2018,(04):933-937.[doi:doi:10.3969/j.issn.1000-4440.2018.04.031]
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白鲜皮中黄柏酮标准样品的研制()
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江苏农业学报[ISSN:1006-6977/CN:61-1281/TN]

卷:
期数:
2018年04期
页码:
933-937
栏目:
加工贮藏·质量安全
出版日期:
2018-08-25

文章信息/Info

Title:
Preparation of certified reference materials of obacunone from bark of Dictamnus dasycarpus Turcz
作者:
耿岩玲; 王晓; 朱姮; 闫慧娇; 宋祥云; 王岱杰
(齐鲁工业大学/山东省科学院/山东省分析测试中心/山东省中药质量控制技术重点实验室，山东济南250014）
Author(s):
GENG Yan-ling; WANG Xiao; ZHU Heng; YAN Hui-jiao; SONG Xiang-yun; WANG Dai-jie
(Qilu University of Technology/Shandong Academy of Sciences/Shandong Analysis and Test Center/Key Laboratory of TCM Quality Control, Jinan 250014, China)
关键词:
黄柏酮; 标准样品; 均匀性; 稳定性; 定值
Keywords:
obacunone; certified reference material; homogeneity; stability; certified value
分类号:
S567
DOI:
doi:10.3969/j.issn.1000-4440.2018.04.031
文献标志码:
A
摘要:
依据GB/T 15000.3-2008标准样品的工作导则，研制黄柏酮标准样品。以白鲜皮为原料，硅胶柱色谱结合重结晶的方法制备黄柏酮单体，通过UV、IR、MS和NMR等技术进行结构表征，同时进行了薄层色谱鉴别和热重分析，通过HPLC检测分析技术，进行了均匀性检验、稳定性检验和8家实验室联合定值。结果表明，该样品均匀性良好，在 0～4 ℃储存24个月稳定性良好，定值结果确定其标准值为98.94%，置信度95%的不确定度为0.12%。说明，黄柏酮标准样品达到了GB/T 15000.3-2008规定的技术要求，具有溯源性，可用于黄柏酮及相关产品的质量控制和检测方法评定。
Abstract:
The certified reference material (CRM) of obacunone was researched according to the technical requirement of general and statistical principle for certification GB/T 15000.3-2008. Using bark of Dictamnus dasycarpus Turcz as material, the obacunone sample was obtained by the method of silica gel chromatography combined with the recrystallization, and the structure was identified by UV, IR, MS and NMR. The purity of obacunone was analyzed by thin-layer chromatography, thermogravimetric and HPLC technology. The samples were investigated by homogeneity test, stability test, and cooperative certification performed by eight laboratories. The results indicated that the obacunone sample had good homogeneity and good stability after storage at 0-4 ℃ for 24 months. The certified value of of obacunone was 98.94% with a expanded uncertainty of 0.12% in confidence level of 95%. The reference material of obacunone was conformed to the technical requirement of GB/T 15000.3-2008 and could be traceable. So, the CRM of obacunone could be used for quality control and test method evaluation of obacunone and related products.

参考文献/References:

[1]国家药典委员会. 中华人民共和国药典. 一部[M]. 北京: 中国医药科技出版社, 2015.
[2]ZHAO W, WOLFENDER J L, HOSTETTMANN K, et al. Antifungal alkaloids and limonoid derivatives from Dictamnus dasycarpus [J]. Phytochemistry, 1998, 47(1): 7-11.
[3]YOON J, PARK M, LEE J H, et al. Endothelial nitric oxide synthase activation through obacunone-dependent arginase inhibition restored impaired endothelial function in ApoE-null mice [J]. Vascular Pharmacology, 2014, 60(3): 102-109.
[4]TANAKA T, MAEDA M, KOHNO H, et al. Inhibition of azoxymethane-induced colon carcinogenesis in male F344 rats by the citrus limonoids obacunone and limonin [J]. Carcinogenesis, 2001, 22(1): 193-198.
[5]TANAKA T, KOHNO H, TSUKIO Y, et al. Citrus limonoids obacunone and limonin inhibit azoxymethane-induced colon carcinogenesis in rats [J]. Bio Factors, 2000, 13(1-4): 213-218.
[6]MURTHY K N C, JAYAPRAKASHA G K, PATIL B S. Obacunone and obacunone glucoside inhibit human colon cancer (SW480) cells by the induction of apoptosis [J]. Food and Chemical Toxicology, 2011, 49: 1616-1625.
[7]MURTHY K N C, JAYAPRAKASHA G K, PATIL B S. Apoptosis mediated cytotoxicity of citrus obacunone in human pancreatic cancer cells [J]. Toxicology in Vitro, 2011, 25(4): 859-867.
[8]KIM J, JAYAPRAKASHA G K, PATIL B S. Obacunone exhibits anti-proliferative and anti-aromatase activity in vitro by inhibiting the p38 MAPK signaling pathway in MCF-7 human breast adenocarcinoma cells [J]. Biochimie, 2014, 105: 36-44.
[9]MURTHY K N C, JAYAPRAKASHA G K, PATIL B S. Cytotoxicity of obacunone and obacunone glucoside in human prostate cancer cells involves Akt-mediated programmed cell death [J]. Toxicology, 2015, 329(2): 88-97.
[10]中国国家质量监督检验总局, 中国国家标准化管理委员会. 标准样品工作导则(2)标准样品常用术语及定义：GB/T 15000.2-94[S]. 北京: 中国标准出版社, 1994.
[11]中国国家质量监督检验总局, 中国国家标准化管理委员会. 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:GB/T 15000.3-2008[S]. 北京: 中国标准出版社, 2008.
[12]SUGIMOTO T, MIYASE T, KUROYANAGI M, et al. Limonoids and quinolone alkaloids from Evodia rutaecarpa Bentham [J]. Chemical and Pharmaceutical Bulletin, 1988, 36 (11)：4453-4461.
[13]中国国家质量监督检验总局, 中国国家标准化管理委员会. 数值修约与极限数值的表示和判定:GB/T 8170-2008[S]. 北京：中国标准出版社，2008.

备注/Memo

备注/Memo:
收稿日期：2017-12-04 基金项目：山东省重大科技创新工程项目（2017CXGC1308）；山东省重点研发计划项目（2017GSF216002、2017CXGC1209）；山东省泰山学者岗位专家支持项目；山东省科学院先导项目 作者简介：耿岩玲（1973-），女，内蒙古呼伦贝尔人，硕士，副研究员，研究方向为天然产物化学及标准样品研制。（E-mail）gengyanling@126.com 通讯作者：王岱杰，（Tel）15965317581；（E-mail）wangdaijie@126.com
更新日期/Last Update: 2018-09-04