摘要
建立了柚皮素标准物质的研制和定值方法。通过红外光谱和核磁共振氢谱对样品进行定性分析,经过柱层析纯化、干燥、混匀后,分装得到120瓶样品。采用质量平衡法和差示扫描量热法进行定值分析(质量平衡法包括液相色谱面积归一化法、水分、无机杂质和残留溶剂的测定)。运用液相色谱法考察了样品的均匀性和稳定性,并对定值结果进行了不确定度评定。结果显示,研制的柚皮素标准物质具有良好的均匀性和稳定性,定值结果为99.2%,扩展不确定度为0.2%,有效期6个月。
A method for preparation and determination of naringenin certified reference material was established.Qualitative analysis of purchased samples was performed using infrared spectroscopy and nuclear magnetic resonance.The samples were purified by column chromatography and dried at 105℃ for 6 h,after mixing and dispensing,120 bottles of reference material candidates were obtained.Purity determination was carried out by differential scanning calorimetry and mass balance method.The mass balance method based on area normalization method of liquid chromatography,included detections on contents of moisture,inorganic impurities and residual solvents.Homogeneity and stability studies were validated by liquid chromatography,and uncertainty of the determination results was also analyzed.Results showed that the developed naringenin certified reference material had good homogeneity and stability,with a purity of 99.2%,an expanded uncertainty of 0.2%(k=2)and a validity period of 6 months.
作者
刘金涛
李玲
董家吏
焦必宁
苏学素
LIU Jin-tao;LI Ling;DONG Jia-li;JIAO Bi-ning;SU Xue-su(College of Chemistry and Chemical Engineering,Southwest University,Chongqing 400715,China;Laboratory of Quality and Safety Risk Assessment for Citrus Product,Ministry of Agriculture and Rural Affairs,Citrus Research Institute,Southwest University/Chinese Academy of Agricultural Sciences,Chongqing 400712,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2020年第2期190-197,共8页
Journal of Instrumental Analysis
基金
国家重点研发专项(2016YFF0201105-2)
国家现代农业(柑桔)产业技术体系建设专项(CARS-26)
国家农产品质量安全风险评估重大专项(GJFP2018004,GJFP2018015)。
关键词
柚皮素
定性分析
标准物质
不确定度
naringenin
qualitative analysis
certified reference materials
uncertainty
