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 for the determination of diacetyl in wine by high performance liquid chromatography (HPLC) with 3,3’-diaminobenzidine (DAB) as derivatization reagent was established. The derivatized products were separated and analyzed by Shim-pack VP-ODS column (250 mm × 4.6 mm, 4.6 μm) using DAB as the derivatization reagent and DAB for 10 min at room temperature. The mobile phase was eluted with a gradient of 0.7 mL / min and measured using a high performance liquid chromatograph with a diode array detector (DAD) at a detection wavelength of 254 nm. The method showed a good linearity in the range of 0.20 ~ 180μmol / L diacetyl with a correlation coefficient (R2) of 0.999, a limit of detection (S / N = 3) of 0.09μmol / N = 10) was 0.20 μmol / L, intraday precision (RSD) was 1.28% (n = 6). The spiked recoveries of real wine samples ranged from 92.0% to 103.6% with RSDs of 0.69% -3.45% (n = 3). The method is simple and quick, the result is accurate and the stability is good. It can be used for the determination of diacetyl in white wine and red wine.