摘要
目的:根据GB/T 15000.3—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》,经国家标准化管理委员会批准立项,研制岩藻甾醇标准样品。方法:选择海带为原料,通过95%乙醇提取、减压浓缩、反复柱色谱分离、石油醚-乙酸乙酯重结晶、残余溶剂去除等制备和纯化过程,获得高纯度岩藻甾醇单体,采用元素分析、红外光谱、质谱、核磁共振和X射线衍射等技术对其进行结构鉴定。运用高效液相色谱-蒸发光散射检测法进行均匀性检验、稳定性检验和8家实验室联合定值检验。结果:该样品在95%置信区间的样品均匀性良好,在2~4℃条件下24个月内稳定性良好,定值测定结果确定其纯度99.54%,扩展不确定度0.16%,达到了国家标准样品的技术要求,通过了国家标准化管理委员会组织的验收。结论:成功研制了岩藻甾醇国家标准样品,该样品可用于岩藻甾醇含量测定、检测方法评定、相关产品的检测与质量控制。
Objective:According to the GB/T 15000.3-2008,to develop a fucosterol certified reference material based on the project approved by Standardization Administration.Method:Fucosterol was isolated from Laminaria japonica dried thallus via 95% ethanol extraction,vacuum concentration,repeated column chromatography separation,recrystallization in petroleum ether-ethyl acetate,and residual solvent removal.Its chemical structure was identified by elemental analysis(EA),infrared spectrum(IR),mass spectrometry(MS),nuclear magnetic resonance(NMR)and X-ray diffraction(XRD).Its homogeneity,stability,and cooperative certification conducted by 8 laboratories were carried out by high performance liquid chromatography with evaporative light scattering detector.Result:For the fucosterol reference material,the certified value of purity was 99.54% with expanded uncertainty of 0.16% in confidence interval of 95%,the stability was good within 24 months storage period at 2-4 ℃,which met the technical requirements of reference material and passed the acceptance organized by Standardization Administration.Conclusion:The national standard materials of fucosterol has been successfully developed,which can be used for the determination of this component,the evaluation of detection methods,and the detection and quality control of related products.
作者
晋文慧
张怡评
陈伟珠
方华
洪专
巢志茂
JIN Wen-hui;ZHANG Yi-ping;CHEN Wei-zhu;FANG Hua;HONG Zhuan;CHAO Zhi-mao(Technology Innovation Center for Exploitation and Utilization of Marine Biological Resources,Third Institute of Oceanography,Ministry of Natural Resources,Xiamen 361005,China;School of Chemical Engineering,Huaqiao University,Xiamen 361021,China;Institute of Chinese Materia Medica,China Academy of Chinese Medical Sciences,Beijing 100700,China)
出处
《中国实验方剂学杂志》
CAS
CSCD
北大核心
2021年第24期131-137,共7页
Chinese Journal of Experimental Traditional Medical Formulae
基金
福建省科技计引导项目(2020N0027)
国家重点研发计划项目(2016YFF0201104)。
关键词
岩藻甾醇
标准样品
均匀性
稳定性
定值
海带
高效液相色谱法(HPLC)
fucosterol
certified reference material
homogeneity
stability
certification
Laminaria japonica dried thallus
high performance liquid chromatography(HPLC)
