三甲基氯硅烷涂层毛细管胶束电动色谱法测定苯甲酸和邻苯二甲酸  

Determination on Benzoic Acid and Phthalic Acid by Micellar Electrokinetic Chromatography with Trimethylchlorosilane-coated Capillaries

作　　者：谢建平[1] 任凯[1] 刘中奎[1] 刘秋艳[1] 邓洪瑞[1] 王晓璐[1] 张亚楠[1] 翟海蝶[1] 

机构地区：[1]周口师范学院,河南周口466001

出　　处：《安徽农业科学》2011年第36期22564-22565,22570,共3页Journal of Anhui Agricultural Sciences

基　　金：河南省高校青年骨干教师资助计划项目(2004162);周口师范学院大学生科研创新基金项目(zknudxs201146);周口师范学院实验室开放项目(201109)

摘　　要：[目的]建立测定苯甲酸和邻苯二甲酸含量的毛细管胶束电动色谱涂层新方法。[方法]采用三甲基氯硅烷涂层的毛细管胶束电动色谱-紫外二极管阵列检测的新方法来分离测定饮料中的苯甲酸和实验室废水中的苯甲酸和邻苯二甲酸,考察了波长、pH值、缓冲介质和电压等因素对苯甲酸和邻苯二甲酸分离测定的影响。[结果]以20 mmol/L SDS+35 mmol/L硼砂(pH值9.5)为运行缓冲液,在检测波长为210 nm,分离电压为14 kV条件下,苯甲酸和邻苯二甲酸在3 min内实现分离,在2～800μg/L范围内两者峰高与浓度有良好的线性关系,其相关系数分别为0.999 3和0.999 9,迁移时间的RSD分别为2.65%和3.69%,峰高的RSD分别是3.12%和4.52%,检出限分别为0.106 7和0.121 3μg/ml。[结论]该测定方法具有试样用量少、操作简捷、灵敏度和准确性好的特点,为防腐剂的分析提供了有效的检测方法。[ Objective ] The study aimed to establish the new method for determining the contents of the benzoic acid and phthalic acid by the micellar electrokinetic chromatography with the coated capillaries. [ Method] The new method of micellar electrokinetic chromatography by using the trimethylchlorosilane coated capillaries with UV diode array detection was used for the separation and determination of benzoic acid in the drink and benzoic acid and phthalic acid in the laboratory waste water. The effects of the wavelength, pH value, buffer solution, voltage and other factors on the separation and determination of the benzoic acid and phthalic acid were investigated. [ Result] Under the optimized operation conditions of 20 mmol/L SDS ＋ 35 mmol/L borate（ pH of 9.5 ）as the running buffer solution, the detection wavelength of 210 nm, and the separation voltage of 14 kV, the benzoic acid and phthalic acid could be separated in 3 min, their good linear relationships between the peak heights and concn, were obtained in the range of 2 - 800 μg/L, with their correlation coefficients being 0. 999 3 and O. 999 9 resp, the RSD of migration time being 2.65% and 3.69% resp. , the RSD of peak height being 3.12% and 4.52%, resp. , and the detection limits being 0. 1067 and 0. 121 3μg/ml resp. [ Conclusion] This new measuring method had the characters of less sample dosage, easy operation and good sensitivity and accuracy, which provided an effective method for the analysis of the preservatives.

关 键 词：胶束电动色谱 涂层 苯甲酸 邻苯二甲酸 三甲基氯硅烷 

分 类 号：TS202.3[轻工技术与工程—食品科学]