白鲜中梣酮标准样品的制备
x

请在关注微信后,向客服人员索取文件

篇名: 白鲜中梣酮标准样品的制备
TITLE:
摘要: 目的:制备梣酮标准样品,确保梣酮及相关产品检测的准确性、可比性和可溯源性。方法:以芸香科植物白鲜的干燥根皮为原料,采用硅胶柱色谱分离制备梣酮单体。分别采用高效液相色谱(HPLC)法、薄层色谱(TLC)法和液质联用(LC-MS)技术对梣酮单体纯度进行分析,通过紫外光谱、红外光谱、质谱和核磁共振等波谱技术对梣酮单体的结构进行表征,并参照GB/T 15000.3标准样品的工作导则要求考察其均匀性、稳定性和定值。结果:HPLC、TLC和LC-MS检测结果显示,所制单体纯度较高,在相关图谱中无明显杂质峰或斑点存在;经多种波谱技术鉴定分离单体化合物为梣酮;所制梣酮单体的均匀性良好,10瓶样品间纯度差异无统计学意义(P>0.05);梣酮单体在0~4 ℃条件下贮藏24个月稳定性良好,稳定性的扩展不确定度为0.16%;8家实验室联合定值试验确定其标准值为99.75%,扩展不确定度为0.34%。结论:成功制备了符合GB/T 15000.3要求的梣酮标准样品,该样品可用于梣酮及相关产品的质量控制和检测方法的评定。
ABSTRACT: OBJECTIVE: To prepare fraxinellone standard sample,and guarantee accuracy,comparability and traceability of fraxinellone and related products. METHODS: Fraxinellone monomer was obtained by means of silica gel chromatography from dried bark of Dictamnus dasycarpus. HPLC,TLC and LC-MS were used to analyze the purity of fraxinellone monomer. Their structures were confirmed by UV,IR,MS and NMR. Homogeneity,stability and constant value of it were investigated by referring to GB/T 15000.3 standard sample. RESULTS: Results of HPLC,TLC and LC-MS showed that the purity of prepared monomer was high. No significant impurity peak or spot was found in related chromatograms. A variety of spectroscopic techniques were used to identify prepared monomeric compound as fraxinellone. Prepared fraxinellone monomer had good uniformity, there was no statistical significance in purity difference among 10 samples(P>0.05). The stability of prepared fraxinellone monomer was good at 0-4 ℃ for 24 months, the extended uncertainty of stability was 0.16%. The standard value of fraxinellone monomer was 99.75% in combination constant value tests of 8 laboratories,and expanded uncertainty was 0.34%. CONCLUSIONS: The fraxinellone was successfully prepared that was conformed to the technical requirement of GB/T 15000.3, and it can be used in the content determination and testing method validation of fraxinellone related products.
期刊: 2018年第29卷第13期
作者: 王岱杰,宋祥云,耿岩玲,付瑞明,于金倩,王晓
AUTHORS: WANG Daijie,SONG Xiangyun,GENG Yanling,FU Ruiming,YU Jinqian,WANG Xiao
关键字: 梣酮;标准样品;均匀性;稳定性;定值;不确定度
KEYWORDS: Fraxinellone; Standard sample; Homogeneity; Stability; Constant value; Uncertainty
阅读数: 55 次
本月下载数: 1 次

* 注:未经本站明确许可,任何网站不得非法盗链资源下载连接及抄袭本站原创内容资源!在此感谢您的支持与合作!