离子色谱法测定维格列汀片中基因毒性杂质氯乙酸含量  

Content Determination of Genotoxic Impurities Chloroacetic Acid in Vildagliptin Tablets by Ion Chromatography

作　　者：母芹 罗誓言 姚诚 杨俊芸 罗东玲 MU Qin;LUO Shiyan;YAO Cheng;YANG Junyun;LUO Dongling(Neijiang Food and Drug Inspection and Testing Center·Sichuan Provincial Drug Administration Key Point of Chemical Quality Control and Evaluation,Neijiang,Sichuan,China 641100)

机构地区：[1]四川省内江市食品药品检验检测中心·四川省药品监督管理局化学药品质量控制及评价重点实验室,四川内江641100

出　　处：《中国药业》2025年第3期76-78,共3页China Pharmaceuticals

基　　金：四川省药品监督管理局科技计划项目[2023001]。

摘　　要：目的建立测定维格列汀片中氯乙酸含量的离子色谱法。方法分析柱为Dionex IonPac AS11-HC阴离子分离柱(250 mm×4.6 mm),保护柱为Dionex IonPac AG11-HC阴离子保护柱(50 mm×4.0 mm),淋洗液为10 mmol/L氢氧化钾溶液,流速为1.0 mL/min,辅助气为99.99%氮气,检测器为抑制电导检测器,检测池温度为35℃,进样量为25μL。结果氯乙酸的质量浓度在0.01~2.00μg/mL范围内与峰面积线性关系良好(r=0.9995,n=7);检测限为11.77 ng/g,定量限为62.77 ng/g;精密度、稳定性试验结果的RSD均小于3.0%;平均加样回收率为101.64%,RSD为4.60%(n=12)。10个厂家的10批样品中,有5批检出氯乙酸杂质,其含量为0.0002%~0.0007%,均低于限度规定的0.0015%。结论该方法操作简便、灵敏度高、专属性强、高效快速,可用于维格列汀片中氯乙酸的含量测定。Objective To establish an ion chromatography(IC)method for the content determination of chloroacetic acid in Vildagliptin Tablets.Methods The analysis column was Dionex IonPac AS11-HC anion separation column(250 mm×4.6 mm),the protection column was Dionex IonPac AG11-HC anion protection column(50 mm×4.0 mm),the eluent was 10 mmol/L suppressed conductivity detector,the flow rate was 1.0 mL/min,the auxiliary gas was 99.99%nitrogen,the detector was the inhibitory conductivity detector,the detection cell temperature was 35℃,and the injection volume was 25μL.Results The linear range of chloroacetic acid was 0.01-2.00μg/mL(r=0.9995,n=7).The limit of detection was 11.77 ng/g and the limit of quantification was 62.77 ng/g.The RSDs of precision and stability test results were all lower than 3.0%.The average recovery rate of chloroacetic acid was 101.64%with an RSD of 4.60%(n=12).Among ten batches of samples from ten manufacturers,impurities of chloroacetic acid were detected in five batches of samples,with the content ranging from 0.0002%to 0.0007%,and all were below the limit of 0.0015%.Conclusion The method is simple,highly sensitive,specific,efficient,and fast,which can be used for the content determination of chloroacetic acid in Vildagliptin Tablets.

关 键 词：离子色谱法 维格列汀片 氯乙酸 基因毒性杂质 含量测定 

分 类 号：R917[医药卫生—药物分析学] R977.15[医药卫生—药学]