2-(乙酰氧基)苯甲酸的HPLC分析方法建立及优化中的几点思考  

Considerations on Establishing and Optimizing an HPLC Method for 2-(acetyloxy)Benzo-ic Acid

作　　者：王娟 范婷婷 刘丰茂[1] Wang Juan;Fan Tingting;Liu Fengmao(College of Science,China Agricultural University,Beijing 100193,China)

机构地区：[1]中国农业大学理学院,北京100193

出　　处：《农药科学与管理》2023年第2期40-46,51,共8页Pesticide Science and Administration

基　　金：农药产品中有效成分含量测定通用分析方法HPLC法。

摘　　要：本文在建立2-(乙酰氧基)苯甲酸的HPLC分析方法过程中,对溶剂对样品的稳定性影响,梯度或等度洗脱的差异,以及特异性参数设置对纯度因子的影响进行了研究。结果表明,在溶剂和流动相中适量加入冰乙酸能有效抑制2-(乙酰氧基)苯甲酸分解为水杨酸;梯度洗脱尽管能产生比等度洗脱峰形更好、峰宽更窄的色谱峰,但梯度洗脱时,流动相中的乙酸会影响方法特异性。方法最终以甲醇和0.1%冰乙酸溶液为流动相,在276 nm的检测波长下,对99%2-(乙酰氧基)苯甲酸原药及30%2-(乙酰氧基)苯甲酸可溶粉剂进行分析。方法确证结果表明该方法满足制剂中2-(乙酰氧基)苯甲酸检测要求。This paper investigates the effect of solvent on the stability of a sample,the differences between gradient or isocratic elution,and the effect of specificity parameter settings on the purity factor in establishing an HPLC method for analyzing 2-(acetyloxy)benzoic acid.The results showed that the decomposition of 2-(acetyloxy)benzoic acid to salicylic acid was effectively inhibited by adding appropriate amounts of glacial acetic acid to the solvent and mobile phase.While gradient elution produced peaks with better peak shape and narrower width than isocratic elution,the acetic acid in the mobile phase during gradient elution could affect the method􀆳s specificity.Finally,the established method was applied to analyze 99%2-(acetyloxy)benzoic acid TC and 30%2-(acetyloxy)benzoic acid soluble powder with methanol and 0.1%glacial acetic acid solution as mobile phases at the detection wavelength of 276 nm.The method validation results showed that the method met the requirements for detecting 2-(acetyloxy)benzoic acid in the formulations.

关 键 词：2-(乙酰氧基)苯甲酸 HPLC 分析方法 

分 类 号：S482.8[农业科学—农药学]