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

引用本文: 王昕洁, 王继宇, 李恒, 惠先, 高文运. 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[J]. 色谱, 2017, 35(8): 837-842. doi: 10.3724/SP.J.1123.2017.04031 shu

Citation: WANG Xinjie, WANG Jiyu, LI Heng, HUI Xian, GAO Wenyun. Determination of diacetyl in liquors by high performance liquid chromatography coupled with precolumn derivatization using 3,3'-diaminobenzidine[J]. Chinese Journal of Chromatography, 2017, 35(8): 837-842. doi: 10.3724/SP.J.1123.2017.04031 shu

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

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
基金项目:
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（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:

English

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

National Engineering Research Center for Miniaturized Detection Systems, College of Life Sciences, Northwest University, Xi'an 710069, China
Received Date: 24 April 2017
Fund Project:
National Natural Science Foundation of China (Nos. 21172179, 21402152)

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:

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

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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

English

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

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中国化学会秘书处

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

English

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

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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通讯作者: 陈斌, bchen63@163.com

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