作者：兰韬¹, 董跟来², 初侨¹, 刘文¹, 杨丽¹, 王鹤妍¹, 王尉³, 席兴军¹

作者单位：1. 中国标准化研究院, 北京 100191;
2. 亚东信基(北京)农产品有限公司, 北京 100125;
3. 北京市理化分析测试中心, 北京 100089

关键词：薯蓣皂素;标准物质;均匀性;稳定性;定值

摘要：

按照JJF 10061994《一级标准物质技术规范》的要求，建立薯蓣皂素标准物质的研制方法。采用IR、UV、MS和NMR等方法对薯蓣皂素标准物质进行定性分析，以高效液相色谱方法进行均匀性和稳定性检验，通过8家实验室的联合定值，完成结果的数据分析。结果表明：该标准物质的均匀性和稳定性良好，定值结果为98.9%，置信度为95%的不确定度为0.2%。研制出的标准物质可用于薯蓣产品的检测和质量控制。

Preparation of Diosgenin certified reference materials

LAN Tao¹, DONG Genlai², CHU Qiao¹, LIU Wen¹, YANG Li¹, WANG Heyan¹, WANG Wei³, XI Xingjun¹

1. China National Institute of Standardization, Beijing 100191, China;
2. Yadongxinji(Beijing) Agricultural Products Co., Ltd., Beijing 100125, China;
3. Beijing Centre for Physical and Chemical Analysis, Beijing 100089, China

Abstract: The preparation method of Diosgenin reference materials was established according to the technical norm of primary reference material(JJF 1006-1994). Qualitative analysis of Diosgenin was carried out by UV, IR, MS and NMR spectrum and high-performance liquid chromatography was carried out for homogeneity and stability inspection. A cooperative certification was conducted with eight laboratories and the certification data were analyzed. The results showed that the homogeneity and stability of Diosgenin were excellent and the certified value was 98.9% with the expand uncertainty of 0.2% in confidence coefficient of 95%. The reference material of Diosgenin can be used for inspection and quality control of related products.

Keywords: Diosgenin;reference material;homogeneity;stability;certification

2017, 43(11): 42-46  收稿日期: 2017-03-18;收到修改稿日期: 2017-05-10

基金项目: 中央基本科研业务费专项经费（562016Y-4687，562016Y-4492，562017Y-5284）；质检公益性行业科研专项项目（201510048-4）

作者简介: 兰韬(1984-),男,安徽马鞍山市人,助理研究员,博士,研究方向为农产品标准样品研制。

参考文献

[1] 李祥,马建中,田广文,等. 薯蓣皂素分析方法综述[J]. 陕西科技大学学报,2009,27(5):163-168.
[2] 汤兴利,徐增莱,夏冰,等. 盾叶薯蓣皂素提取工艺及检测方法研究进展[J]. 中药材,2004,27(11):877-880.
[3] 王博. 具有抗肿瘤活性薯蓣皂素衍生物的合成及作用机制的研究[D]. 沈阳:沈阳药科大学,2012.
[4] 李辉,倪晋仁. 薯蓣皂甙元的研究进展[J]. 精细化工,2010, 27(1):60-65.
[5] 王天伦. 黄姜的综合利用[D]. 湘潭:湖南科技大学,2015.
[6] 张文秀. 薯蓣皂苷元对人宫颈癌细胞增殖的影响[J]. 中国现代医生,2011,(26):5-7.
[7] LEE M S, YUET-WA J C, KONG S K, et al. Effects of polyphyllin D, a steroidal saponin in paris polyphylla, in growth inhibition of human breast cancer cells and in xenograft[J]. Cancer Biology & Therapy,2005,4(11):1248-1254.
[8] LEPAGE C, LIAGRE B M, PINON A. Cyclooxygenase-2 and 5-lipoxygenase pathways in diosgenin-induced apoptosis in HT-29 and HCT-116 colon cancer cells[J]. International Journal of Oncology,2010,36(5):1183-1191.
[9] 郭剑伟,苏丽娜,刘光明. 薯蓣皂素提取工艺研究进展[J].中国药业,2011,20(18):13-16.
[10] 张裕卿,王东青,李滨县,等. 阶梯生物催化协同提取盾叶薯蓣中薯蓣皂苷元的研究[J]. 中草药,2006,37(5):688-691.
[11] 张雯,李成涛,王少伟. 生物法提取薯蓣皂素工艺研究[J].中国酿造,2008,194(17):54-55.
[12] 毛楠,黄文,籍国东,等. 分离-发酵法提取皂素清洁工艺研究[J]. 环境工程,2009(27):177-180.
[13] 王尉,周晓晶,乐胜锋,等. 白藜芦醇标准样品的研制[J].中国测试,2015,41(4):39-42.
[14] 标准物质定值的通用原则及统计学原理:JJF 1343-2012[S].北京:中国质检出版社,2012.
[15] AGRAWAL P K, JAIN D C, AIN R K, et al. Carbon-13 NMR spectroscopy of steroidal sapogenins and steroidal saponins[J]. Phytochemistry,1985,24(11):2479-2496.