高效液相色谱法测定蜜饯中柠檬黄的不确定度评定  

Uncertainty Evaluation Determination of Lemon Yellow in Preserves by High Performance Liquid Chromatography

作　　者：张慧琼 郑陆红 陈嘉敏 ZHANG Huiqiong;ZHENG Luhong;CHEN Jiamin(Guangdong Provincial Public Laboratory of Food Industry,Guangzhou 511442,China;Guangdong Food Industry Institute Co.,Ltd.,Guangzhou 511442,China;Guangdong Quality Supervision Food Inspection Statio,Guangzhou 511442,China)

机构地区：[1]广东省食品工业公共实验室,广东广州511442 [2]广东省食品工业研究所有限公司,广东广州511442 [3]广东省质量监督食品检验站,广东广州511442

出　　处：《现代食品》2022年第23期195-198,208,共5页Modern Food

摘　　要：目的:建立一种高效液相色谱法测定蜜饯中柠檬黄含量的不确定度分析方法,找出影响不确定度的相关因素,对不确定度进行计算,如实反映测量的置信度和准确度。方法:试验样品采用聚酰胺吸附法提取,制成水溶液,采用phenomenex C18色谱柱(250 mm×4.6 mm,5μm)分离,流动相以甲醇为A相,以0.02 mol·mL^(-1)乙酸铵溶液为B相,梯度洗脱,二极管阵列检测器检测,并用峰面积外标法来定量。考察实验过程中,各种影响实验结果的可能因素,建立数学模型,评定各个不确定度分量,计算合成相对标准不确定度和扩展不确定度。结果:本实验测得蜜饯中的柠檬黄含量为0.035 g·kg^(-1)时,取置信水平p=95%(k=2),扩展不确定度为0.001 g·kg^(-1)(k=2),其结果可表示为(0.035±0.001)g·kg^(-1)。测定过程中的不确定度来源有标准溶液配制、样品称量、试样定容体积、试样稀释倍数等。结论:本方法可反映测量的置信度和准确性,为采用高效液相色谱法测定蜜饯中柠檬黄含量提供可靠的理论依据。Objective:To establish an uncertainty analysis method for the determination of lemon yellow content in candied fruit by high performance liquid chromatography,to find out the factors affecting the uncertainty,to evaluate the uncertainty,to give the uncertainty,and to faithfully reflect the confidence and accuracy of the measurement.Method:The test samples were extracted by polyamide adsorption method,made into an aqueous solution,separated by phenomenex C18column(250 mm×4.6 mm,5μm),the mobile phase was methanol as the A phase,0.02 mol·L^(-1)ammonium acetate solution was used as the B phase,gradient elution,diode array detector detection,and quantified by peak area external standard method.Investigate the various possible factors affecting the experimental results in the experimental process,establish mathematical models,evaluate each uncertainty component,and calculate the relative standard uncertainty and extended uncertainty of synthesis.Result:When the yellow content of lemon in the candied fruit was 0.035 g·kg^(-1),the confidence level p=95%(k=2)and the expansion uncertainty was 0.001 g·kg^(-1)(k=2),and the result could be expressed as(0.035±0.001)g·kg^(-1).Sources of uncertainty in the determination process include standard solution preparation,sample weighing,specimen volume,specimen dilution multiple,etc.Conclusion:This method can reflect the confidence and accuracy of the measurement,and provide a reliable theoretical basis for the determination of lemon yellow content in candied fruit by high performance liquid chromatography.

关 键 词：柠檬黄 高效液相色谱法 蜜饯 不确定度评定 

分 类 号：S202.3[农业科学—农业工程]