芳香族羧酸的高效液相色谱法测定及其在药品分析中的应用  

Determination of Aromatic Carboxylic Acids by High Performance Liquid Chromatography and Its Application in Pharmaceutical Analysis

作　　者：董影杰[1] 于泓[1] 张小东 

机构地区：[1]哈尔滨师范大学化学化工学院,黑龙江哈尔滨150025 [2]黑龙江省齐齐哈尔矿产勘查开发总院,黑龙江齐齐哈尔161006

出　　处：《分析测试学报》2010年第6期564-567,572,共5页Journal of Instrumental Analysis

基　　金：黑龙江省教育厅科学技术研究项目(10551103);哈尔滨师范大学科技发展预言项目(08XYG-15)

摘　　要：建立了反相高效液相色谱同时测定苯甲酸、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ZORBAX ODS反相色谱柱为分离柱,采用紫外检测方法,研究了流动相组成、淋洗梯度和检测波长对芳香族羧酸分离效果的影响。在优化色谱条件下,即流动相为乙酸水溶液（50 mmol.L-1,pH3.5）-甲醇（60∶40）,紫外检测波长为230 nm,流速为1.0 mL.min^-1,色谱柱温度为30℃,6种芳香族羧酸在25 min内达到基线分离。方法的检出限为0.21-0.99 mg.L-1,平均加标回收率为99.7%-100.1%,相对标准偏差小于0.60%。将方法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,结果满意。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,salicylate acid,phthalic acid,p-hydroxy salicylate acid,p-amino benzoic acid and o-methyl benzoic acid.The separation of the six aromatic carboxylic acids was performed on a ZORBAX ODS column（250 mm × 4.6 mm i.d.,5 μm）.The quantitation analysis of six aromatic carboxylic acids was carried out by ultraviolet（UV） detection.Influences of composition of mobile phase,elution gradient and detection wavelength on the separation and determination of six aromatic carboxylic acids were investigated.The optimum chromatographic conditions were as the follows： mobile phase： acetic acid aqueous solution（50 mmol·L-1,pH 3.5）-methanol（60∶40,by volume）,detection wavelength： 230 nm,flow rate： 1.0 mL·min^-1,column temperature： 30 ℃.The six aromatic carboxylic acids were successfully separated in 25 min.The calibration curve showed a good linearity over the tested range for the six aromatic carboxylic acids with correlation coefficients of 0.999 9.The detection limits ranged from 0.21 to 0.99 mg·L-1.The average recoveries were in the range of 99.7%-100.1%with RSDs less than 0.60%.The method was applied in the determinination of six aromatic carboxylic acids in Zujunqing Tinctura and Salicylic Acid and Benzoic Acid Terpineol Liniment samples with satisfactory results.

关 键 词：高效液相色谱法 芳香族羧酸 药品 紫外检测 

分 类 号：O657.72[理学—分析化学] Q946.828.3[理学—化学]