岩藻黄质标准样品的研制  

Development of Fucoxanthin Certified Reference Material

作　　者：张怡评[1,2] 陈伟珠[1] 方华[1] 谢全灵[1] 陈晖[1] 洪专[1] 易瑞灶[1] 吴皓[2] 

机构地区：[1]国家海洋局第三海洋研究所,福建厦门361005 [2]南京中医药大学,南京210023

出　　处：《化学分析计量》2015年第6期1-5,共5页Chemical Analysis And Meterage

基　　金：福建省科技计划重大专项专题项目(2013NZ0003);福建省科技计划重点项目(2013NZ0015);海洋公益性行业科研专项(201405017)

摘　　要：研制了岩藻黄质标准样品。以海带为原料,通过提取、分离纯化制备高纯岩藻黄质,采用红外光谱(IR)、高分辨质谱(MS)和核磁共振谱(NMR)进行结构确证。样品分装成150瓶样品后,采用高效液相色谱–紫外检测法进行均匀性、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%的置信区间范围内样品均匀性良好;在–18℃条件下,进行24个月长期稳定性考察,结果表明样品在24个月内稳定性良好;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,岩藻黄质标准样品定值结果为99.53%,相对扩展不确定度为0.22%(k=1.96)。该标准样品达到标准样品的技术要求,可用于有关岩藻黄质相关产品的方法校正和质量控制。Fucoxanthin certified reference material was developed. Fucoxanthin was made from the Laminaria japonica. The structure of fucoxanthin certified reference material was comfirmed by infrared spectroscopy （IR）, high resolution mass spectral（MS） and nuclear magnetic resonance（NMR）. Fucoxanthin was divided into 150 bottles. The homogeneity and stability testing and quantitative analysis were carried out by high performance liquid chromatography- ultraviolet detector （HPLC-UV）. According to analysis procedure of homogeneity, 15 bottles of sample were randomly taken from 150 bottles, and the results were validated by F test statistical methods. The stability inspection was carried within 24 months, and the results indicated that the period for fucoxanthin of storage was 24 months at -18℃. A cooperative certification was conducted with 8 qualified laboratories. The certified purity value of the reference material of fucoxanthin was 99.53% with a relative expaned uncertainty of 0.22%（k=1.96）. The reference material 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 fucoxanthin.

关 键 词：岩藻黄质 标准样品 均匀性 稳定性 定值 不确定度 

分 类 号：O656[理学—分析化学]