D-甘露醇标准样品的研制  

Development of D-mannitol certified reference material

作　　者：晋文慧 陈伟珠 张怡评 方华 洪专 蒋声铸 巢志茂[3] JIN Wen-hui;CHEN Wei-zhu;ZHANG Yi-ping;FANG Hua;HONG Zhuan;JIANG Sheng-zhu;CHAO Zhi-mao(Technology Innovation Center for Exploitation of Marine Biological Resources,the Third Institute of Oceanography,Ministry of Natural Resources,Xiamen Fujian 361005;Xiamen Tasman Bio-tech Co.,Ltd.,Xiamen Fujian 361021;Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700)

机构地区：[1]自然资源部第三海洋研究所,自然资源部海洋生物资源开发利用工程技术创新中心,福建厦门361005 [2]厦门塔斯曼生物工程有限公司,福建厦门361021 [3]中国中医科学院中药研究所,北京100700

出　　处：《中南药学》2021年第12期2639-2644,共6页Central South Pharmacy

基　　金：福建省科技计引导项目(No.2020N0027);福建省海洋经济发展资金项目(No.2019-2021;FJHJF-L-2021-4);国家重点研发计划项目(No.2016YFF0201104)。

摘　　要：目的通过国家标准化管理委员会批准立项,研制D-甘露醇标准样品。方法 采用海带为原料,通过95%乙醇提取、减压浓缩、低温析晶、反复水溶、脱色、热过滤、重结晶、残余溶剂去除等制备和纯化过程,获得高纯D-甘露醇单体,采用元素分析,旋光性分析,红外光谱,质谱和核磁共振技术对其进行结构鉴定。并通过高效液相色谱蒸发光散射检测分析技术,进行均匀性、稳定性和8家实验室联合定值检验。结果该样品在95%CI内样品均匀性良好,在2~4℃条件下,24个月内稳定性良好,定值测定结果确定其特性标准值为(99.84±0.12)%(置信度95%,k=2),达到了国家标准样品的技术要求。结论成功研制了D-甘露醇国家标准样品,可用于D-甘露醇含量测定、检测方法评定、相关产品的检测与质量控制。Objective To develop a D-mannitol certified reference material by Standardization Administration of the People’s Republic of China.Methods D-mannitol was prepared from Laminaria japonica Aresch via 95% ethanol extraction,vacuum concentration,repeated column chromatography separation,recrystallization of petroleum ether-ethyl acetate,and residual solvent removal.Its chemical structure was identified by elemental analysis,optical activity analysis,infrared spectrum,mass spectrum,and nuclear magnetic resonance methods.Its homogeneity,stability,and cooperative certification by 8 laboratories were systematically checked by high performance liquid chromatography with an evaporative light-scattering detector.Results The homogeneity and stability of D-mannitol reference material were good,and the certified purity of the reference material was (99.84±0.12)% (95% confidence level,k=2).The stability was good within 24 months storage period at 2-4℃.The reference material of D-mannitol conformed to directives for the work guide of reference materials.Conclusion The national reference material of D-mannitol is developed successfully,which can be used for the determination of D-mannitol content,the evaluation of detection methods,and the detection and quality control of related products.

关 键 词：D-甘露醇 标准样品 均匀性 稳定性 定值 海带 

分 类 号：R284[医药卫生—中药学]