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四烯菌素B标准样品的研制

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目的:依据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》,研制四烯菌素B标准样品。方法:以淀粉酶产色链霉菌(Streptomyces diastatochramogenes)1628发酵液为原料,通过萃取、AB-8和SephardexLH-20柱层析分离纯化得四烯菌素B纯品。利用紫外(UV)、红外(IR)、质谱(MS)和核磁图谱(NMR)分析,查阅文献数据,进行结构确认。样品分装成100瓶(10 mg/瓶),结合液相色谱法对该样品展开均匀性、稳定性检验以及联合定值分析。结果:该样品经F检验在95%的置信区间范围内均匀性良好;在-20~-18 ℃条件下保存12个月稳定性良好;经国内8家具有分析资质的实验室协同定值,四烯菌素B纯度为99。37%,扩展不确定度为0。22%。结论:四烯菌素B达到国家标准样品的技术要求,可用于有关四烯菌素B的检测方法校准和相关产品的质量控制。
Development of certified reference material of tetrin B
Aims:This paper aims to develop a certified reference material(CRM)of tetrin B according to GB/T 150003-2008"Guidelines for the Work of Standard Samples(3)General Principles and Statistical Methods for Determining the Value of Standard Samples".Methods:Tetrin B was obtained from metabolites of Streptomyces diastatochramo genes 1628 by extraction,AB-8 and Sephardex LH-20 column chromatography.The structure of tetrin B was confirmed by UV,IR,MS and NMR analysis.Subsequently,tetrin B was divided into 100 bottles with 10 mg per bottle.The homogeneity and stability testing and cooperative certification were carried out by HPLC detection.Results:The homogeneity was good within 95% confidence interval by the F test statistical method.The sample was stable within a 12 months storage period at-20~-18 ℃.A cooperative certification was conducted with 8 qualified laboratories;and the certified purity value of tetrin B 99.37% with an expanded uncertainty of 0.22% .Conclusions:The reference material tetrin B conforms to the technical requirement of the certified reference material.The material can be used in the method validation and quality control regarding tetrin B.

tetrin Bstandard sampleuniformitystabilityuncertainty

雷承泽、刘一鹏、申屠旭萍、俞晓平

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中国计量大学生命科学学院浙江省生物计量及检验检疫技术重点实验室,浙江杭州 310018

四烯菌素B 标准样品 均匀性 稳定性 不确定度

国家重点研发计划项目浙江省领雁计划项目浙江省三农九方科技协作项目

2022YFF06079052022C020472023SNJF034

2024

中国计量大学学报
中国计量学院

中国计量大学学报

CHSSCD
影响因子:0.357
ISSN:2096-2835
年,卷(期):2024.35(2)