HPLC测定奥格列汀中基因毒性杂质残留量_郑飞.pdfVIP

HPLC 测定奥格列汀中基因毒性杂质残留量  * 郑飞，华国栋 (北京中医药大学东方医院药学部，北京 100078) 摘要：目的 建立奥格列汀原料药中基因毒性杂质的HPLC 测定方法。方法 采用Zorbax SB-C18 色谱柱(250 mm× 4.6 mm ， 5 µm) ，进样量：20 μL；流动相为0.1% 乙酸水- 乙腈(65 ∶35)；流速为1 mL·min1；紫外检测器，检测波长为220 nm；柱 温为25 ℃，色谱乙腈为溶剂。结果 该方法专属性良好，测得苯磺酸异丙酯在4~60 μg·mL1 内线性关系良好，平均回 收率为98.56%(n=9 ，RSD=3.78%) ，溶液在8 h 内稳定。结论 该法操作简便，重复性好，结果准确可靠，可用于奥格列 汀原料药中基因毒性杂质的测定。 关键词：奥格列汀；原料药；基因毒性杂质；苯磺酸异丙酯；高效液相色谱法 中图分类号：R917.101 文献标志码：B 文章编号：1007-7693(2017)03-0396-03 DOI: 10.13748/ki.issn1007-7693.2017.03.020 Determination of Genotoxic Impurities in Omarigliptin by HPLC * ZHENG Fei, HUA Guodong (Department of Pharmacy, Dongfang Hospital of Beijing University of TCM, Beijing 100078, China) ABSTRACT: OBJECTIVE To establish an HPLC method to determine genotoxic impurities in omarigliptin bulk drug. METHODS The HPLC was carried out with Zorbax SB-C18 column with the column temperature of 25 ℃. The injection volume was 20 μL. The mobile phase was 0.1% acetic acid water solutiom-acetonitrile (65 ∶35) with the flow rate of 1 1 mL·min . The detector was UVD with the detection wave of 220 nm. Acetonitrile was used as solvent for omarigliptin. RESULTS Isopropyl benzenesulfonate could be separated completely with good linear relationship in 460 µg·mL1. The average recovery of isopropyl benzenesulfonate was 98.56%(n=9, RSD=3.78%). CONCLUSION This method is simple, reproducible and accurate for determination of genotoxic impurities in omarigliptin bulk drug. KEY WORDS: omarigliptin; bulk drug; genotoxic impurities; isopropyl benzenesulfonate; HPLC 奥格列汀为超长效二肽基肽酶-4(DPP-4)抑制 有关物质杂质 Y01 、Y02(北京康悦药业，批号分 剂，其作用机制是通过抑制体内 DPP-4 酶对胰高