有机酸的非抑制型离子排斥色谱法测定  

Determination of Organic Acids by Ion-exclusion Chromatography with Non-suppressed Conductivity Detection

作　　者：原小寓[1] 吴伟[2] 于泓[1] 

机构地区：[1]哈尔滨师范大学化学系 [2]黑龙江大学化学化工与材料学院,黑龙江哈尔滨150080

出　　处：《分析测试学报》2008年第1期76-78,83,共4页Journal of Instrumental Analysis

基　　金：黑龙江省教育厅科学技术研究项目(10551103)

摘　　要：研究了非抑制型离子排斥色谱分离测定7种有机酸（柠檬酸、酒石酸、苹果酸、琥珀酸、乳酸、甲酸、乙酸）的方法。以Shim—pack SCR-102H柱为分离柱，选用对甲苯磺酸-乙腈为淋洗液，考察了淋洗液浓度、流速、pH、色谱柱温度及淋洗液中乙腈含量等条件对分离和测定的影响。通过实验确定最佳的色谱条件：2．0mmol／Lp-甲苯磺酸-乙腈（体积比91：9）为淋洗液，流速1．0mL／min，柱温50℃，pH2．8。该法对所测有机酸的检出限在0．06～1．05mg／L之间，相对标准偏差在3．3％以下（n=5），加标回收率在96％～101％之间，整个分析过程在11min内完成。A method was developed for the separation and determination of seven organic acids, viz citric acid, tartaric acid, malic acid, succinic acid, lactic acid, formic acid and acetic acid by ionexclusion chromatography with non-suppressed conductivity detection. Chromatographic separation of the acids was performed on a Shim-pack SCR-102H column（ 80 × 30 mm i. d. ）at 50 ℃, and eluted with a mixture of 2.0 mmol/L p-toluenesulfonic acid and acetonitrile. The effects of the concentration of the eluent, the temperature of the chromatographic column, and the acetonitrile concentration in the eluent on the retention time of organic acids were investigated. Under optimum conditions, the organic acids could be separated and determined simultaneously in 11 min. The detection limits（ S/N = 3 ） of the organic acids ranged from 0. 06 to 1.05 mg/L. The relative standard deviations ranged from 0. 9% to 3.3%（n=5, measuring peak area） and the recoveries ranged from 96% to 101%. The method has been applied to the determination of the organic acids in apple juice with satisfactory resuits.

关 键 词：离子排斥色谱法 有机酸 非抑制型电导检测 

分 类 号：O657.75[理学—分析化学] Q946.81[理学—化学]