四烯菌素B标准样品的研制

Development of certified reference material of tetrin B

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。

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 diastatochramogenes 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.