固相萃取-反相高效液相色谱法同时测定浓缩果汁中的11种有机酸

Simultaneous determination of 11 organic acids in concentrated juices using SPE-reverse-phase high performance liquid chromatography

建立了反相高效液相色谱（RP-HPLC）同时测定果汁中酒石酸、奎宁酸、苹果酸、莽草酸、Vc、乙酸、马来酸、乳酸、琥珀酸、富马酸以及柠檬酸的方法。样品直接用水稀释后,再经C18固相萃取柱分离后,采用Aichrom BondAQC18（25cm×4.6mm,粒径5μm）色谱柱分离,二极管阵列检测器检测,外标法定量。以0.02mol/LNH4H2PO4溶液（pH2.8）-甲醇（体积比为99：1）为流动相,在0.8mL/min下等度洗脱,于210nm波长下检测。1次可以同时测定果汁中的11种有机酸,有机酸的标准曲线相关系数均在0.9900以上,回收率在85.1%~95.5%之间,对苹果汁、草莓汁、梨汁以及石榴汁中的有机酸进行了分析检测,该方法杂质干扰小,回收率高、重现性好,能够对苹果汁、草莓汁、梨汁以及石榴汁中的有机酸进行准确的定性定量分析。

A method was developed for the determination of the tartaric acid,quinic acid,malic acid,shikimic acid,Vc,acetic acid,maleic acid,lactic acid,succinic acid,fumaric acid and citric acid in juices using reversephase high performance liquid chromatography.The sample was diluted by water and then was purified by C18 solid-phase extraction（SPE）.Reverse-phase liquid chromatographic analysis was performed on the instrument of Agilent 1100 series equipped with a diodearray detector and autosampler.The column was Aichrom BondAQ C18（25 cm×4.6 mm,5 μm）.The mobile phase was 0.02 mol/L NH4H2PO4（pH2.8）-Methanol（99：1,v/v） with a flow rate of 0.8 mL/min.The detection wavelength was 210 nm.The retention time for all of organic acids in the pear,apple,strawberry and pomegranate juices were less than 15 min after the samples treated by SPE.The calibration curve for the organic acids was in good linearity with a correlation coefficient of upwards 0.990.The recovery ratio of the organic acids was 85.1%~95.5% and the coefficient of variation was less 4%.The results indicate that this method is handy,fast,veracious and practical for the routine analysis of organic acids in juices.