Lin Xiaojie, Wei Wei, He Zhigang, Lin Xiaozi
Se Pu. 2014 Mar;32(3):304-8. doi: 10.3724/sp.j.1123.2013.11023.
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 x 7.8 mm, 7 microm) was used at 50 degrees C. 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 microL. 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 0.999 7 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.
建立了一种同时测定黄酒中有机酸的离子排斥色谱法。采用IC-Pak离子排斥柱（300 mm×7.8 mm，7μm），柱温50℃。流动相为硫酸（A相）和乙腈（B相）（98:2，v/v），流速为0.5 mL/min。梯度洗脱程序如下：0～40 min，0.01 mol/L硫酸至0.02 mol/L硫酸；40～50 min，0.01 mol/L硫酸。进样量为10μL。检测波长设定为210 nm。结果表明，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、异丁酸和丁酸在30 min内可完全分离并测定。在0.001～1.000 g/L范围内，线性相关系数均大于0.999 7。在优化条件下，黄酒中有机酸的回收率在93.4%～103.8%之间，相对标准偏差（RSD，n = 5）为0.1%～1.5%。该方法可行、简便、快速、准确，适用于黄酒中有机酸的定量分析。
