反相高效液相色谱法测定α-[(二甲基氨基)亚甲基]-β-酮基-2-噻吩丙腈  

RP-HPLC Determination of α-[(Dimethylamino)Methylene]-β-keto-2-Thiophenepropanonitrile

作　　者：刘妍如[1,2] 黄荣清[1] 肖炳坤[1] 杨建云[1] 黄洪林[2] 

机构地区：[1]军事医学科学院放射与辐射医学研究所,北京100850 [2]江西中医学院,南昌330004

出　　处：《理化检验（化学分册）》2011年第2期157-159,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家自然科学基金项目(No.20672143);国家科技重大专项"重大新药创制"综合性新药研究开发技术大平台(2009zx09301-002)

摘　　要：应用反相高效液相色谱法测定α-[(二甲基氨基)亚甲基]-β-酮基-2-噻吩丙腈(IDP-3)的含量。采用Phenomex C18色谱柱(4.6 mm×250 mm,5μm),并以不同比例混合的甲醇和水的混合溶液作梯度淋洗;检测波长为330 nm,外标法定量。在优化的色谱条件下,IDP-3与其它共存物质能够良好地分离。IDP-3的质量浓度在10.0～100 mg.L-1范围内与峰面积呈线性关系,检出限(3S/N)及测定下限(10S/N)分别为0.01 mg.L-1和0.035 mg.L-1。精密度试验表明,日内相对标准偏差(n=6)在0.43%～0.64%之间。A method for the determination of α-[（dimethylamino） methylene]-β-keto-2-thiophenepropanonitrile（abbreviated as IDP-3） by RP-HPLC was proposed.IDP-3 and its by-products were separated on Phenomex C18 column（4.6 mm×250 mm,5 μm）,using a mixture of methanol and water mixed in different ratios as mobile phase in the gradient elution.External standard calibration was adopted in the determination at the wavelength of 330 nm.It was found that under the optimum condition,IDP-3 was well separated from the co-existing substances.Linear relationship between values of peak area and concentration of IDP-3 was obtained in the range of 10.0-100 mg·L-1,with values of detection limit（3S/N） and lower limit of determination（10S/N） of 0.01 mg·L-1 and 0.035 mg·L-1 respectively.Test for precision was made,and values of intraday RSD′s（n=6） found were in the range of 0.43%-0.64%.

关 键 词：反相高效液相色谱法 -α[(二甲基氨基)亚甲基]-β-酮基-2-噻吩丙腈 梯度淋洗 

分 类 号：O652.63[理学—分析化学]