木霉素标准样品的研制  

Development of certified reference material of trichodermin

作　　者：朴怡情 申屠旭萍[1] 叶子弘[1] PIAO Yiqing;SHENTU Xuping;YE Zihong(Zhejiang Key Laboratory of Biometrology,Inspection and Quarantine,China Jiliang University,Hangzhou 310018,China)

机构地区：[1]中国计量大学浙江省生物计量及检验检疫技术重点实验室

出　　处：《中国计量大学学报》2019年第4期484-489,共6页Journal of China University of Metrology

基　　金：国家重点研发计划项目(No.2016YFF0202300);浙江省重点研发计划项目(No.2018C02030,2019C02015);杭州市科技计划项目(No.20190101A01)

摘　　要：目的:依据GB/T15000.3-2008《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》,在国家标准化管理委员会批准立项的基础上,研制木霉素标准样品。方法:以脐孢木霉菌代谢产物为原料,通过提取及硅胶柱层析分离到木霉素纯品,采用紫外光谱(UV)、红外光谱(IR)、质谱(MS)和核磁共振(NMR)对其进行结构确认。样品分装成100瓶(10 mg/瓶)后,采用气相色谱法进行了均匀性检验、稳定性检验和联合定值分析。结果:经F检验该样品在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进行协同定值,木霉素纯度定值结果为99.86%,扩展不确定度为0.05%。结论:本研究所得的木霉素达到国家标准样品的技术要求,可用于有关木霉素的检测方法校正和质量控制。Aims: This paper aims to develop a certified reference material(CRM) of trichodermin according to the Directives for CRM General and Statistical Principle for Certification(GB/T 15000. 3-2008) based on the CRM project approved by the Standardization Administration of the People’s Republic of China(SAC). Methods: Trichodermin was obtained from the metabolite of Trichoderma brevicompactum by extraction and silica gel column chromatography. The structure of trichodermin was confirmed by UV, IR, MS and NMR analysis. Subsequently, trichodermin was divided into 100 bottles with 10 mg per bottle. The homogeneity and stability testing and cooperative certification were carried out by gas chromatography detection. Results: The homogeneity was good within 95% confidence interval by the F-test statistical method. The sample was stable within 12 months storage period at-20^-18 ℃. A cooperative certification was conducted with 8 qualified laboratories and the certified purity value of trichodermin was 99.86% with an expanded uncertainty of 0.05%. Conclusions: The reference material trichodermin can conform to the technical requirement of the certified reference material. The material is intended for use in the method validation and quality control regarding trichodermin.

关 键 词：计量 木霉素 标准样品 均匀性 稳定性 定值 不确定度 

分 类 号：TB195.6[一般工业技术]