Development of a Certified Reference Material for Lyophilized Vitamin K1
ZHANG Xiao-guang1,HUANG Ting2,ZHANG Wei2,HUANG Liang3, QUAN Can2,LI Hong-mei2,YANG Yi1
1. College of Science, Beijing University of Chemical Technology, Beijing 100029, China;
2. National Institute of Metrology, Beijing 100029, China;
3. Guangzhou Institute of Measuring and Testing Technology, Guangzhou, Guangdong 510030, China
Abstract：Dimethyl sulfone (DMSO) is firstly applied as the solvent for a lyophilized certified reference material (CRM). Vitamin K1/DMSO solution is prepared by gravimetry, and is sub-divided and lyophilized, the lyophilized vitamin K1 CRM is developed through qualitative analysis, quantitative analysis, homogeneity study, stability study and uncertainty evaluation. Certified value of lyophilization vitamin K1 is analyzed by high performance liquid chromatography method, using the vitamin K1 purity CRM as a calibrant. The certified value is 0.96 mg/mL, with the relative expanded uncertainty of 7%. The method of CRM lyophilized vitamin K1 makes great significance for the accurate determination the disease in clinical examination and the long-term preservation of vitamin K1.
［1］李向荣,方晓,陈青俊,等. 反相液相色谱法同时测定食物中维生素K1和K2［J］.营养学报,1988, 20 (1): 72-75.
［2］李云巧,王东冬.稀土溶液标准物质的研制［J］.计量学报,2003, 24 (4): 348-351.
［3］马联弟,王晶,曹文祺,等. 粮食中营养成分标准物质制备技术［J］.计量学报,2004, 25(3):275-277.
［4］杨梦瑞,戴新华,杨屹,等.冰冻人血清尿酸标准物质的研制［J］.计量学报,2010, 31(1):86-90.
［5］Boss E A, Filho R M, Coseelli E. Freeze drying process: real time model and optimization ［J］. Chemical Engineering and Processing, 2004, 43 (12):1475-1485.
［6］International Organization for Standardization ISO, Reference materials—General and statistical principles for certification［S］.
［6］ISO Guide 35:2006. Reference materials－General and statistical principles for certification［S］.
［7］Véronique D, Mickael P, Francois L, et al. Quantitative determination of plasma vitamin K1 by high-performance liquid chromatography coupled to isotope dilution tandem mass spectrometry［J］.Journal of analytical biochemistry, 2010, 401 (1) : 7-14.
［8］Qin X S, Ai D W, Li D, et al. HPLC-APCI-MS for the determination of vitamin K1 in human plasma: Method and clinical application［J］. Journal of Chromatography B, 2008, 875 (2) : 541-545.
［9］National Institute of Advanced Industrial Science and Technology (AIST), Japan, Spectral Database for Organic Compounds［DB］. http://sdbs.db.aist.go.jp/sdbs/cgi-bin/direct_frame_top.cgi, 2014-03-14.
2015, Vol. 36 
