角鲨烯国家标准样品的研制

Development of Squalene Certified Reference Material

为研制角鲨烯国家标准样品。以角鲨烯粗品为原料,制备高纯角鲨烯,采用红外光谱、高分辨质谱和核磁共振谱进行结构确证。样品分装成150瓶后,采用气相色谱-氢火焰离子化检测器法进行均匀性、稳定性检验和定值分析。从样品中随机抽取15瓶进行均匀性检验,经F检验表明在95%置信区间范围内样品均匀性良好;稳定性考察按照-18℃长期实验稳定性(24个月)进行,结果表明在考察期间内样品稳定性良好;标准样品经国内8家具有分析资质的实验室进行协同定值,并评定了定值结果的不确定度,角鲨烯标准样品定值结果为99.57%,相对扩展不确定度为0.30%(k=1.96)。该标准样品达到国家标准样品的技术要求,可用于有关角鲨烯的方法校正和质量控制。

Squalene certified reference material was developed by purification of crude squalene. The structure of the certified reference material was confirmed by infrared spectroscopy(IR), high resolution mass spectrometry(HRMS) and nuclear magnetic resonance(NRM) and squalene was divided into 150 aliquots. The homogeneity and stability tests and quantitative analysis were carried out by gas chromatography-flame ionization detection(GC-FID). Fifteen randomly selected aliquots showed good homogeneity as indicated by F-test analysis at a 95% confidence interval. The test samples were stable at-18 ℃ for 24 months. A cooperative certification was conducted with 8 qualified laboratories. The certified purity value of the reference material was 99.57% with a relatively expanded uncertainty of 0.30%(k = 1.96). The reference material can conform to the technical requirement of the certified reference material. This material was intended for use in the method validation and quality control regarding squalene.