水果中主要有机酸的离子排斥色谱法测定条件研究  

Study on the Condition of Determination of Main Organic Acids in Fruits by Ion Exclusion Chromatography

作　　者：庞荣丽[1] 成昕 方金豹[1] 谢汉忠[1] 郭琳琳[1] 

机构地区：[1]中国农业科学院郑州果树研究所/农业部果品及苗木质量监督检验测试中心,郑州450009 [2]农业部农产品质量安全中心监督处,北京100081

出　　处：《食品工业》2015年第4期261-266,共6页The Food Industry

基　　金：中国农业科学院创新工程科技经费项目(CAAS-ASTIP-2015-ZFRI);河南省大宗水果产业技术体系资助

摘　　要：为研究水果果实中有机酸组分的测定方法,以草莓、桃、葡萄等水果为试材,电导检测模式下,采用离子排斥色谱,对流动相类型、柱温、流动相浓度、流动相流速等色谱条件进行了优化试验,并按照国家有关检测方法标准的要求,利用优化后的色谱条件,对不同有机酸标准曲线相关性、线性范围、准确度等方法技术参数进行了测试。由有资质的5家实验室对方法的重复性和再现性进行了不同实验室间的比对试验。结果表明,适宜的色谱条件为采用专用有机酸色谱柱（ICSep COREGEL-64H）,柱温为65℃,流动相浓度为5.0 mmol/L的硫酸溶液,流动相流速为0.60 m L/min,抑制器再生液为0.1 mol/L的氯化锂溶液。在该条件下,有机酸各组分分离效果佳,不同有机酸标准曲线相关性好（相关系数r在0.999 5和1.000 0之间）,线性范围广（分别为柠檬酸0.000 5~0.400 0 g/L、苹果酸0.000 2~0.200 0 g/L、酒石酸0.000 2~0.200 0 g/L、琥珀酸0.000 2~0.100 0 g/L）,方法定量限低（分别为柠檬酸0.010 0 g/kg,酒石酸、苹果酸、琥珀酸均为0.004 0 g/kg）,准确度高（回收率范围为80%~110%）,重复性和再现性好,适合水果中有机酸组分的定量测定。In order to study the determination method of organic acid composition of fruits, using strawberry, peach, grape etc as test material, with conductance detection mode, chromatographic conditions of ion exclusion chromatOgraphy including mobile phase type, column temperature, mobile phase concentration, mobile phase flow rate etc were optimized. In accordance with the requirements of national related standard test methods of the technical parameters by using the method of the optimized chromatographic conditions （standard curve, linearity range, accuracy etc.） were tested. The method repeatability and repttxtuobility were tested by 5 laboratories accredited. The results showed that the optimum chromatographic condition was that using special organic acid chromatography column （ICSep COREGEL-64H）, the column temperature of 65 ℃, mobile phase concentration of sulfuric acid solution of 5.0 mmol/L, flow rate of 0.60 mL/min, suppressor regeneration liquid lithium chloride solution of 0.1 mol/ L. Underlhis coxtilion, separation effect was goed, and different organic acid standard curve conelation was good（r between 0.9995 and 1.0000）. The wide linearity range （citric acid 0.000 5,-0.400 0 g/L, malic acid 0.000 2-0.200 0 g/L, tartaric acid 0.000 2--0.200 0 g/L, succinate acid 0.000 2-0.100 0 g/L）, low methods quantitative limit （respectively citric acid 0.010 0 g/kg, tartaric acid, malic acid and succinic acid were 0.004 0 g/kg）, high accuracy （recovery rate was 80%--110%）, high repeatability and reproducibility were observed. This method was suitable for determination of organic acids in fruits.

关 键 词：离子排斥色谱 电导检测 有机酸 水果 

分 类 号：TS255.7[轻工技术与工程—农产品加工及贮藏工程] O657.7[轻工技术与工程—食品科学与工程]