【作者】 董影杰；

【导师】 于泓；

【作者基本信息】 哈尔滨师范大学 ， 分析化学， 2011， 硕士

【摘要】 开展了高效液相色谱法分析芳香族羧酸及离子液体的应用研究,目的是建立简单、准确、快速和污染小的分析芳香族羧酸的方法,同时拓展离子液体在液相色谱分析中的应用。第一,建立了反相高效液相色谱同时分离测定苯甲酸、水杨酸、邻苯二甲酸、对羟基苯甲酸、对氨基苯甲酸和邻甲苯甲酸6种芳香族羧酸的方法。以反相色谱柱为分离柱,采用紫外检测方法,研究了紫外检测波长、流动相组成和淋洗梯度对分离和测定芳香族羧酸的影响。在最佳色谱条件下,6种芳香族羧酸达到基线分离,整个分离过程在25 min内完成。方法的检出限为0.21～0.99 mg/L。将方法应用于足君清酊剂和水杨酸苯甲酸松油搽剂两种药品的分析,平均加标回收率为99.7%～100.1%,相对标准偏差小于0.6%,结果表明本方法简便快捷,准确可靠。第二,建立了以离子液体作高效液相色谱流动相添加剂测定水杨酸的方法。实验以反相色谱柱为分离柱,采用紫外检测方法,研究了紫外检测波长、离子液体烷基链长度、离子液体溶液的浓度以及pH值等对分离和测定的影响,并与其它分析水杨酸的方法进行了对比实验。在最佳色谱条件下,水杨酸的保留时间约为4.4 min,检出限为0.059 mg/L。将方法应用于足菌清酊剂药品的分析,平均加标回收率为99.9%,相对标准偏差为0.11%。本方法结果准确、可靠、重复性好,适用于相关药品和食品的质量控制分析。第三,建立了以离子液体作流动相添加剂同时分离测定氨基苯甲酸异构体(邻氨基苯甲酸、间氨基苯甲酸、对氨基苯甲酸)的高效液相色谱分析方法。实验以反相色谱柱为分离柱,采用紫外检测方法,考察了检测波长、离子液体烷基链长度、离子液体溶液的浓度以及pH值等对分离和测定的影响。在最佳色谱条件下,三种氨基苯甲酸在4 min内达到基线分离,检出限为0.045～0.077 mg/L。本方法被成功应用于药品溴米娜普鲁卡因注射液中对氨基苯甲酸含量的测定。平均加标回收率为99.8%～100%；相对标准偏差均小于0.2%。第四.建立了四甲基铵根离子的高效液相色谱-间接紫外检测分析法。以反相色谱柱为分离柱,采用间接紫外检测方法,考察了紫外检测波长和离子液体+有机溶剂(乙腈、甲醇)流动相对分离和测定四甲基铵根离子的影响。在最佳色谱条件下,四甲基铵根离子的保留时间约为5.9 min,检出限为2.60 mg/L。将本方法应用于分析离子液体溴化四甲基铵中的四甲基铵根离子,其平均加标回收率为99.27%,相对标准偏差为0.24%,结果令人满意。更多还原

【Abstract】 An investigation into analysis of aromatic carboxylic acids as well as the application of ionic liquids in high performance liquid chromatography was carried out. The purpose of this research is to establish simple, accurate, fast and less contaminative methods to determine aromatic carboxylic acids and to develop the application of ionic liquids in high performance liquid chromatography.Firstly, an analytical method based on reverse phase high performance liquid chromatography was established for the simultaneous separation and determination of six aromatic carboxylic acids, including benzoic acid, salicylic acid, phthalic acid, p-amino benzoic acid, p-hydroxyl salicylic acid and o-methyl benzoic acid. The separation of the six aromatic carboxylic acids was performed on a ZORBAX ODS column. The detection of the six aromatic carboxylic acids was carried out by ultraviolet (UV) detection. The influences of composition of mobile phase, elution gradient and detection wavelength on the separation and determination of the six aromatic carboxylic acids were investigated. Under the optimum chromatographic conditions, the six aromatic carboxylic acids were successfully separated in 25 min. The detection limits of the tested components were from 0.21 to 0.99 mg/L. The method has been used to determine two kinds of pharmaceutical. Recoveries of spiked components were between 99.7% and 100.1%. and the relative standard deviations were less than 0.6%.Secondly, an analytical method based on reverse phase high performance liquid chromatography was established for the determination of salicylic acid. The chromatographic separation of salicylic acid was performed on a ZORBAX ODS column. The detection of salicylic acid was carried out by ultraviolet (UV) detection. The comparison of three different mobile phases was performed. The effects of detection wavelength, concentrations, pH value and length of alkyl chain on different ionic liquids on the separation and determination of salicylic acid were investigated. Under the optimum chromatographic conditions, the retention time of salicylic acid was about 4.4 min. The detection limit of salicylic acid was 0.059 mg/L. The method has been successfully used to determine the content of salicylic acid in the pharmaceutical of Zujunqing Tinctura. The average recovery of spiked component was 99.9%, and the relative standard deviation was 0.11%.Thirdly, an analytical method based on reverse phase high performance liquid chromatography was established for the separation and determination of the isomers of amino benzoic acid, including o-, m-,p-amino benzoic acid, and the essential feature of the method is that 1-alkyl-3-methylimidazolium salts are used as mobile phase additives. The separation of the o-, m-,p-amino benzoic acid was performed on a ZORBAX ODS column. The detection of the o-, m-,p-amino benzoic acid was carried out by ultraviolet (UV) detection. The effects of the detection wavelength, pH value, length of alkyl chain on different ionic liquids, and the concentrations on the separation and determination of these analytes were performed. Under the optimum chromatographic conditions, the o-, m-,p-amino benzoic acid were successfully separated within 4 min. The detection limits of the o-, m-,p-amino benzoic acid were from 0.045 to 0.077 mg/L. The method has been successfully used to determine the content of p-amino benzoic acid in the pharmaceutical of Bromine mitag Procaine Injection. Recoveries of spiked components were between 99.8% and 100%, and the relative standard deviations were less than 0.2 %.Finally, a method was developed for the determination of tetramethyl ammonium ion by reverse phase high performance liquid chromatography with indirect ultraviolet (UV) detection. Chromatographic separation was performed on a ZORBAX ODS reverse phase column and chromatographic detection was carried out by indirect UV detection using ionic liquids+organic solvents (acetonitrile or methanol) as mobile phase. The effects of the ultraviolet detection wavelength and mobile phases on the separation and determination of tetramethyl ammonium ion were investigated. Under the optimum chromatographic conditions, the retention time of tetramethyl ammonium ion was about 5.9 min. The detection limit of tetramethyl ammonium ion was 2.60 mg/L. The method has been applied to the determination of tetramethyl ammonium ion in ionic liquid tetramethyl ammonium bromide. The recovery of tetramethyl ammonium ion after spiking was 99.27%. and the relative standard deviation was 0.24%.更多还原