柱前衍生化反相高效液相色谱法测定盐酸二甲双胍缓释片中二甲胺含量  

Content Determination of Dimethylamine in Metformin Hydrochloride Sustained-Release Tablets by RP-HPLC with Pre-Column Derivatization

作　　者：张一平 张倩 王一然 宫晓菲 任雅丽 夏学军[1] 刘玉玲[1] ZHANG Yiping;ZHANG Qian;WANG Yiran;GONG Xiaofei;REN Yali;XIA Xuejun;LIU Yuling(Institute of Materia Medica,Chinese Academy of Medical Sciences and Peking Union Medical College·Beijing Key Laboratory of Drug Delivery Technology and Novel Formulations,Beijing,China 100050;The Place PharmaceuticalCo.,Ltd.,Yancheng,Jiangsu,China 224100)

机构地区：[1]中国医学科学院北京协和医学院药物研究所·药物传输技术及新型制剂重点实验室,北京100050 [2]世贸天阶制药<江苏>有限责任公司,江苏盐城224100

出　　处：《中国药业》2020年第21期44-48,共5页China Pharmaceuticals

摘　　要：目的建立测定盐酸二甲双胍缓释片中二甲胺含量的柱前衍生化反相高效液相色谱法。方法样品经2,4-二硝基氟苯衍生化,采用高效液相色谱法分析,色谱柱为XDB-C18柱(150 mm×4.6 mm,5μm),流动相为0.1%磷酸溶液(A)-乙腈(B),梯度洗脱(0 min时40%B,12 min时55%B,13.2 min时75%B,18 min时40%B),检测波长为380 nm,流速为1.2 m L/min,柱温为30℃。结果二甲胺质量浓度在0.2~0.6μg/m L范围内与峰面积线性关系良好(r=0.9991);检测限为4.59 ng/m L,定量限为17.80 ng/m L;平均加样回收率为98.00%,RSD为1.37%(n=9)。结论该方法灵敏度高、易于操作,可用于盐酸二甲双胍缓释片中二甲胺含量的测定。Objective To establish a reversed phase high performance liquid chromatography(RP-HPLC)method with pre-column derivatization for the content determination of dimethylamine in Metformin Hydrochloride Sustained-Release Tablets.Methods The samples were derivatized by 2,4-dinitrofluorobenzene and analyzed by the HPLC method.The chromatographic column was XDB-C18 column(150 mm×4.6 mm,5μm),the mobile phase was 0.1%phosphoric acid solution(A)-acetonitrile(B),gradient elution(0 min40%B;12 min,55%B;13.2 min,75%B;18 min 40%B),the detection wavelength was 380 nm,the flow rate was 1.2 m L/min,and the column temperature was 30℃.Results The dimethylamine showed good linear relationship with peak area in the range of 0.2-0.6μg/m L(r=0.9991).The limit of detection was 4.59 ng/m L and the limit of quantification was 17.80 ng/m L.The average recovery rate was 98.00%,and the RSD was 1.37%(n=9).Conclusion The method is sensitive and easy to operate,which can be used for the content determination of dimethylamine in Metformin Hydrochloride Sustained-Release Tablets.

关 键 词：衍生化法 高效液相色谱法 盐酸二甲双胍缓释片 二甲胺 含量 

分 类 号：R927.2[医药卫生—药学] R977.15