色谱

色谱 ›› 2017, Vol. 35 ›› Issue (8): 837-842.DOI: 10.3724/SP.J.1123.2017.04031

• 研究论文 • 上一篇    下一篇

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

王昕洁, 王继宇, 李恒, 惠先, 高文运   

  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
  • 收稿日期:2017-04-24 出版日期:2017-08-08 发布日期:2013-11-25
  • 通讯作者: 高文运E-mail:gaowenyun@nwu.edu.cn
  • 基金资助:

    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）.

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

WANG Xinjie, WANG Jiyu, LI Heng, HUI Xian, GAO Wenyun   

  1. National Engineering Research Center for Miniaturized Detection Systems, College of Life Sciences, Northwest University, Xi'an 710069, China
  • Received:2017-04-24 Online:2017-08-08 Published:2013-11-25
  • Supported by:

    National Natural Science Foundation of China (Nos. 21172179, 21402152); Natural Science Foundation of Educational Department of Shaanxi Province (No. 15JK1710).

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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（250 mm×4.6 mm，4.6 μ m）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0.20~180 μ mol/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0.09 μ mol/L，定量限（S/N=10）为0.20 μ mol/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。

关键词: 3, 3'-二氨基联苯胺, 高效液相色谱, 酒, 双乙酰, 柱前衍生

Abstract:

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 μ m) 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 μ mol/L to 180 μ mol/L with the correlation coefficient (R2) of 0.999. The limit of detection (S/N=3) and limit of quantification (S/N=10) were 0.09 μ mol/L and 0.20 μ mol/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 from 92.0% 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.

Key words: 3,3'-diaminobenzidine (DAB), diacetyl, high performance liquid chromatography (HPLC), liquors, pre-column derivatization

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