1. 哈尔滨师范大学化学化工学院
2. 哈尔滨石油学院
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王婧菲, 于泓, 卜文. 离子液体作高效液相色谱流动相添加剂分离测定芳香族羧酸[J]. 分析测试学报, 2014,33(5):533-538.
Determination of Aromatic Carboxylic Acids by High Performance Liquid Chromatography with Ionic Liquids as Mobile Phase Additives[J]. 2014,33(5):533-538.
以离子液体作反相高效液相色谱流动相添加剂,建立了分离测定对氨基苯甲酸、邻苯二甲酸、对羟基苯甲酸、水杨酸、苯甲酸、邻甲苯甲酸6种芳香族羧酸的方法。以C18反相色谱柱为分离柱,采用紫外检测方法,以离子液体作高效液相色谱流动相添加剂,考察了检测波长、甲醇含量、离子液体溶液的pH值、离子液体烷基链长度以及离子液体溶液浓度等分离及测定条件。优化得到的色谱条件为:以甲醇和 1.0 mmol/L 1-丁基-3-甲基咪唑四氟硼酸盐水溶液(pH 3.0)(体积比40∶60)为流动相;检测波长240 nm;流速1.0 mL/min;柱温30 ℃。在优化条件下对6种芳香族羧酸进行梯度洗脱,约在16.5 min内分离完全;在5~120 mg/L范围内,线性系数均在0.999以上;检出限为0.026~0.082 mg/L。方法的平均加标回收率为98.3%~103.8%,相对标准偏差不高于0.63%。将该方法应用于药品复方紫荆皮水杨酸溶液和足君清酊剂中芳香族羧酸的测定,结果满意。
A reversed-phase high performance liquid chromatographic method was developed for the determination of six aromatic carboxylic acids including p-amino benzoic acid,phthalic acid,p-hydroxy benzoic acid,salicylate acid,benzoic acid and o-methyl benzoic acid,by using ionic liquids as mobile phase additives.The chromatographic separation of aromatic carboxylic acids was performed on a RP-C18 column.The detection of aromatic carboxylic acids was carried out by ultraviolet(UV) detection.The comparison of three different mobile phases was performed.When the ionic liquids were chosen as mobile phase additives,the chromatogram was improved with better chromatographic peak shape and higher sensitivity.Effects of experimental conditions,e.g.detection wavelength,methanol content,pH value,concentrations and alkyl chain length of ionic liquids on separation and determination of aromatic carboxylic acids were investigated.The optimum chromatographic conditions were as follows:mobile phase:methanol-1.0 mmol/L 1-butyl-3-methylimidazolium tetrafluoroborate aqueous solution(pH 3.0)(40∶60),UV detection wavelength:240 nm,flow rate:1.0 mL/min,column temperature:30 ℃.The six aromatic carboxylic acids were successfully separated within 16.5 min under the optimal conditions.The calibration curves showed good linearities over the range of 5-120 mg/L for aromatic carboxylic acids with correlation coefficients more than 0.999.The average recoveries of spiked components were in the range of 98.3%-103.8%,with relative standard deviations not more than 0.63%.The method was successfully used to determine the content of aromatic carboxylic acids in pharmaceuticals,Compound Redbud Bark and Salicylic Acid solution and the Zujunqing Tinctura.
离子液体高效液相色谱法芳香族羧酸紫外检测药品
ionic liquidhigh performance liquid chromatography(HPLC)aromatic carboxylic acidsultraviolet detectionpharmaceutical
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