离子排斥色谱法测定黄酒中的13种有机酸

建立了离子排斥色谱法（ion-exclusion chromatography，IEC）测定黄酒中有机酸含量的分析方法。使用Waters离子排斥色谱柱（300 mm×7.8 mm，7 μm），流动相为H₂SO₄溶液（A）与乙腈（B）的混合溶液（体积比为98：2），线性梯度程序：0~40 min，流动相A的浓度由0.01 mol/L 上升到0.02 mol/L；40~50 min，流动相A的浓度为0.01 mol/L ；流速为0.5 mL/min，柱温50 ℃，进样量10 μL，检测波长210 nm。结果表明，该方法可在30 min内实现草酸、马来酸、柠檬酸、酒石酸、苹果酸、抗坏血酸、琥珀酸、乳酸、富马酸、乙酸、丙酸、异丁酸和丁酸的完全分离与定量，13种有机酸在0.001~1.000 g/L范围内线性关系良好，回归方程的线性相关系数在0.9997以上。黄酒中13种有机酸的加标回收率为93.4%~103.8%，相对标准偏差为0.1%~1.5%（n=5）。该方法简单快捷、准确、重复性好，可用于黄酒中有机酸的测定。

Determination of organic acids in rice wine by ion-exclusion chromatography

An ion-exclusion chromatographic method for the simultaneous determination of organic acids in rice wine was developed. An IC-Pak Ion Exclusion column (300 mm×7.8 mm, 7 μm) was used at 50 ℃. The mobile phases were H₂SO₄(phase A) and acetonitrile (phase B) (98:2, v/v) at a flow rate of 0.5 mL/min. The gradient elution program was as follows: 0-40 min, 0.01 mol/L H₂SO₄ to 0.02 mol/L H₂SO₄; 40-50 min, 0.01 mol/L H₂SO₄. The injection volume was 10 μL. The detection wavelength was set at 210 nm. The results showed that oxalic acid, maleic acid, citric acid, tartaric acid, malic acid, ascorbic acid, succinic acid, lactic, fumaric acid, acetic acid, propionic acid, isobutyric acid and butyric acid were completely separated and determined in 30 min. The linear correlation coefficients were above 0.9997 in the range of 0.001-1.000 g/L. Under the optimized conditions, the recoveries of organic acids in rice wine were in the range of 93.4%-103.8% with the relative standard deviations (RSDs, n=5) of 0.1%-1.5%. This method is feasible, convenient, fast, accurate and applicable for the quantitative analysis of the organic acids in rice wine.