离子色谱/直接电导法测定利格列汀药物中三氟乙酸残留  

Determination of Trifluoroacetic Acid( TFA) Residues in Linagliptin Drugs by Ion Chromatography with Direct Conductance

作　　者：周长朋 王东武 郑文凤 许洁 徐利娜 

机构地区：[1]迪沙药业集团国家认定企业技术中心质量研究院,山东威海264205

出　　处：《分析测试学报》2015年第12期1425-1429,共5页Journal of Instrumental Analysis

摘　　要：建立了离子色谱/直接电导法测定利格列汀药物中三氟乙酸残留的方法。利格列汀药物经二氯甲烷溶解后加水进行萃取,水相过滤膜后直接进样。采用EGⅢ在线发生20 mmol/L氢氧化钾溶液为淋洗液,以Ionpac AS11-HC（4 mm×25 cm）色谱柱及Ionpac AG11-HC（4 mm×5 cm）保护柱进行分离,流速为1.2 m L/min,ASRS 500-4 mm阴离子抑制器和电导检测器抑制并直接检测,抑制电流60 m A,柱温30℃,进样体积25μL。结果表明,三氟乙酸与碳酸根离子及其他成分的分离度良好,三氟乙酸在0.848～6.46μg/m L范围内线性关系良好（r=0.999 4）,检出限（LOD）为0.031 8μg/m L,定量下限（LOQ）为0.106μg/m L。该方法操作简单、灵敏度高、重现性好,可用于利格列汀药物中三氟乙酸残留的检测。An ion chromatographic method was developed for the determination of trifluoroacetic acid（ TFA） residues in linagliptin drugs. After dissolved with dichlomethane and extracted with water,the samples were loaded onto the instument. The determination was performed on an Ionpac AS11-HC（ 4 mm × 25 cm） column with an Ionpac AG11-HC（ 4 mm × 5 cm） guard column. The eluent was 20 mmol / L potassium hydroxide solution produced on-line with EGⅢ KOH at a flow rate of 1. 2m L / min. TFA was detected by suppressed conductivity with an ASRS 500-4 mm suppressor at a current of 60 m A. The column temperature was set at 30 ℃ and the injection volume was 25 μL.There was a good resolution between trifluoroacetic acid and other components. The calibration curve showed a good linearity（ r = 0. 999 4） in the range of 0. 848-6. 46 μg / m L. The limit of detection（ LOD） was 0. 031 8 μg /m L and the limit of quantitation（ LOQ） was 0. 106 μg /m L. The method has the advantages of simple operation,high sensitivity and good reproducibility,and could be used for the detection of trifluoroacetic acid（ TFA） residues in linagliptin drugs.

关 键 词：离子色谱-直接电导法 三氟乙酸 利格列汀 

分 类 号：O657.75[理学—分析化学] TQ460.72[理学—化学]