3,3'-二氨基联苯胺柱前衍生高效液相色谱法测定酒中双乙酰  

Determination of diacetyl in liquors by high performance liquid chromatography coupled with precolumn derivatization using 3,3′-diaminobenzidine

作　　者：王昕洁[1] 王继宇[1] 李恒[1] 惠先[1] 高文运[1] 

机构地区：[1]西北大学国家微检测系统工程研究中心,生命科学学院,陕西西安710069

出　　处：《色谱》2017年第8期837-842,共6页Chinese Journal of Chromatography

基　　金：国家自然科学基金项目(21172179,21402152);陕西省教育厅自然科学基金项目(15JK1710)~~

摘　　要：以3,3′-二氨基联苯胺(DAB)为衍生化试剂,建立了柱前衍生高效液相色谱测定酒中双乙酰含量的分析方法。双乙酰与衍生化试剂DAB在室温条件下反应10 min进行柱前衍生,并采用Shim-pack VP-ODS色谱柱(250mm×4.6 mm,4.6μm)对衍生化产物进行分离分析,以水-甲醇为流动相进行梯度洗脱,流速为0.7 mL/min,并采用配有二极管阵列检测器(DAD)的高效液相色谱仪测定,检测波长为254 nm。该法在双乙酰浓度为0.20~180μmol/L的范围内呈现良好的线性关系,相关系数(R2)为0.999,检出限(S/N=3)为0.09μmol/L,定量限(S/N=10)为0.20μmol/L,日内精密度(RSD)为1.28%(n=6)。实际酒样品的加标回收率为92.0%~103.6%,RSD为0.69%~3.45%(n=3)。该法简便快捷,结果准确,稳定性好,可以用于白酒及红酒中双乙酰含量的测定。A method was developed for the determination of diacetyl in liquors by high performance liquid chromatography-ultraviolet(HPLC-UV)coupled with precolumn derivatization using derivatization reagent 3,3′-diaminobenzidine(DAB). Diacetyl reacted with DAB at room temperature for 10 min. Then the separation was carried out on a high performance liquid chromatograph equipped with a diode array detector(DAD). A Shim-pack VP-ODS(250 mm×4. 6 mm,4. 6 μm)column was employed using water-methanol mobile phases for gradient at a flow rate of 0. 7 mL/min and detection wavelength of 254 nm. The method showed a good linearity at diacetyl concentrations from 0. 20 μmol/L to 180 μmol/L with the correlation coefficient(R2)of 0. 999. The limit of detection(S/N = 3)and limit of quantification(S/N = 10)were 0. 09μmol/L and 0. 20 μmol/L,respectively. The intra-day precision(RSD)was 1. 28%(n = 6). The method was further evaluated in the analysis of liquor samples with the recoveries ranging from92. 0% to 103. 6% and RSDs from 0. 69% to 3. 45%(n = 3). The method is well suitable for the measurement of diacetyl in liquor samples.

关 键 词：高效液相色谱 柱前衍生 3 3' -二氨基联苯胺 双乙酰 酒 

分 类 号：O658[理学—分析化学]