摘要
以7-氨基-1,3-萘二磺酸为柱前衍生试剂,采用邻氯苯甲酸为内标,建立了苯甲酸及其单取代物的区带毛细管电泳-二极管阵列检测器(DAD)分离测定方法。实验考察了运行缓冲液浓度及pH值,β-CD浓度、柱温及分离电压对分离的影响。优化实验条件下,苯甲酸及其单取代衍生物峰面积与内标物峰面积之比与分析物相应浓度呈良好线性关系,相关系数是0.9972～0.9998,样品加标回收率在97.6%～101.5%之间,相对标准偏差为0.68%～2.04%。采用该法对实际生抽、老抽样品中的苯甲酸进行测定,结果满意。
A novel, rapid and highly efficient method for the separation of benzoic acid and its mono- substituted benzoic acid derivatives by capillary zone electrophoresis has been developed. To optimize operational conditions,the background electrolyte concentration, column temperature, voltage and other factors were evaluated. The optimum conditions were as follows.30 mmol/L borate buffer at pH 9.5,15 mmol/Lβ-CD and column temperature at 20 ℃. The applied voltage was 18 kV and detection wavelength was set at 254 nm. Under the optimum conditions, 10 derivatives of benzoic acid and its mono-substituted benzoic acids were completely separated with a good baseline resolution. The detection limits（at a signalto-noise ratio of 3） were in the range of 0. 01-0. 03 μg/mL. The linear ranges were from 1.01 to 140.1 μg/mL. The established method was rapid, simple and effective for the determination of the content of benzoic acid from the extracted light soy sauce and dark soy sauce with sotisfactory results.
出处
《分析科学学报》
CAS
CSCD
北大核心
2013年第2期291-293,共3页
Journal of Analytical Science
关键词
苯甲酸
苯甲酸取代物
柱前衍生
Benzoic acid
Substituted benzoic acid
Pre-column derivatization
作者简介
白新伟，男，硕士，助教，主要从事毛细管电泳技术的应用研究．
