血清中尿酸和尿素含量测定的超高效液相色谱–单四级杆质谱法国际比对  

Determination of Uric Acid and Urea in Serum by Ultra Performance Liquid Chromatography–Single Quadrupole Mass Spectrometry for International Comparison

作　　者：石莲花 金有训 何海红[1] 全灿[1] 徐蓓[1] 李红梅[1] Shi Lianhua;Jin Youxun;He Haihong;Quan Can;Xu Bei;Li Hongmei(National Institute of Metrology, Beijing　100029, China)

机构地区：[1]中国计量科学研究院,北京100029

出　　处：《化学分析计量》2017年第4期85-88,共4页Chemical Analysis And Meterage

基　　金：国家科技基础专项(2011FY130100);国家重点研发计划项目(2016YFD0500800);中国计量科学研究院比对专项(03-AJLSF15)

摘　　要：基于单四极杆质谱建立了血清中尿酸、尿素含量准确测定的同位素稀释超高效液相色谱–质谱方法,并以该方法参加了国际物质量咨询委员会(CCQM)组织的"血清中尿酸尿素含量测定"的K、P国际比对。血清样品用乙腈除去蛋白质,分别采用C18反相柱和电喷雾(ESI)负离子模式检测尿酸、CN正相柱和ESI正离子模式检测尿素,同位素稀释的单点校准法进行定量,用3种标准物质(GBW 09157,GBW 09169,NIST SRM 909c)进行方法验证,测量比对血清样品(Ⅰ,Ⅱ)获得国际等效一致性。该方法操作简单、快速准确,适用于血清中尿酸尿素的定量分析。The method to determine uric acid and urea in serum was established by single quadrupole-based isotope dilution ultra performance liquid chromatography-mass spectrometer,which was used for CCQM-K and P international comparison.Acetonitrile was added in the sample for protein precipitation,a C18reversed-phase column and electrospray ionization(ESI)negative ion mode was used to determine uric acid,and CN normal-phase column and ESI positive ion mode were used to determine urea,and a single point calibration method for quantitative isotope dilution.This method was verified with GBW09157,GBW09169and NIST SRM909c certified reference materials,and serum samples(Ⅰ,Ⅱ)were measured to obtain international equivalent consistency.The method is simple in operation,rapid and accurate,it is suitable for quantitative analysis of urea in serum uric acid.

关 键 词：单四级杆质谱 同位素稀释液相色谱–质谱法 尿酸 尿素 血清 国际比对 

分 类 号：O657.7[理学—分析化学]