摘要
为验证检验机构的毛细管电泳检测能力及进行毛细管电泳检测能力比对,按照JJF 1059.1—2012《测量不确定度评定与表示》、CNAS-GL05:2011《测量不确定度要求的实施指南》及CNAS-GL06:2006《化学分析中不确定度的评估指南》,对新开发的毛细管电泳电化学发光检测鱼露中的L-羟脯氨酸含量的不确定度进行评定。不确定度来源主要有标准溶液、移取定容体积、试样重复测定、回收率和最小二乘法拟合标准曲线。结果表明,该方法中最小二乘法拟合标准曲线求试样含量引入的不确定度u_c对合成标准不确定度的贡献最大,其次为试样重复测定引入的不确定度u_(rep),而L-羟脯氨酸标准溶液配制过程中引入的不确定度u_s也不容小觑。上述3个方面应该在实验过程中加以注意,以提高实验的准确度。本研究对各个不确定度分量进行量化,得出鱼露中的L-羟脯氨酸含量为(50.44±8.80)mg/L,k=2.576。研究结果为L-羟脯氨酸含量测定新方法的质量控制提供了理论依据。
In order to verify the ability of capillary electrophoresis of the inspection body and compare the ability of capillary electrophoresis,the uncertainty evaluation of the new method for detection of L- hydroxyproline in fish sauce through capillary electrophoresis electrochemiluminescence was conducted in accordance with JJF 1059. 1—2012 " Evaluation and Expression of Uncertainty in Measurement",CNAS- GL05: 2011 " Guidance on the Application of the Requirements for Measurement Uncertainty" and CNAS- GL06: 2006 " Guidance on Evaluating the Uncertainty in Chemical Analysis". After the analysis of L- hydroxyproline measurement,the uncertainty sources included standard solution,pipetting volume by volume,repetitive sample measurement,recovery and least- squares fitting standard curve. The results showed that in the L- hydroxyproline detection method,the uncertainty ucintroduced for the measurement of content by the least square method to fit the standard curve contributes highest to combined standard uncertainty,followed by uncertainty urepintroduced for repeated measurement. Furthermore,the uncertainty usintroduced for the L- hydroxyproline standard solution preparation process should not be underestimated. Attention should be paid to the above three aspects in the experiment process,in order to improve the accuracy of the experiment.Through each quantified uncertainty components on fish sauce,the results showed that L- hydroxyproline content was( 50. 44 ± 8. 80) mg /L,k = 2. 576. The research results provide a theoretical basis for the quality control of new determination methods of L- hydroxyproline content.
出处
《中国渔业质量与标准》
2016年第4期31-36,共6页
Chinese Fishery Quality and Standards
基金
诏安县质量计量检验检测所事业发展基金〔2016〕004号
关键词
毛细管电泳
电化学发光
L-羟脯氨酸
不确定度
鱼露
capillary electrophoresis
electrochemiluminescence
L-hydroxyproline
uncertainty
fish sauce