反相高效液相色谱法测定N-｛3-［3-(二甲基氨基)-1-氧基-2-丙烯基］-苯基｝乙酰胺及其相关物质  

RP-HPLC Determination of N-{3-[3-(Dimethylamino)-1-oxo-2-propenyl]-phenyl} Acetamide and Its Interrelated Substances

作　　者：李科研[1] 黄荣清[1] 肖炳坤[1] 杨建云[1] 李良[1] 段卫华 

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]总参管理保障部中心门诊部药局,北京100082

出　　处：《理化检验（化学分册）》2010年第3期283-285,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

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

摘　　要：N-{3-[3-(二甲基氨基)-1-氧基-2-丙烯基]-苯基}乙酰胺(NDAOPPAM)样品用流动相甲醇-水(38+62)混合溶液溶解,用DiamonsilC18色谱柱作固定相。在所述条件下,NDAOPPAM与合成反应中的反应物之一,3-乙酰氨基苯乙酮(AAMPAN)可完全分离。定量中用紫外光谱检测,波长为236nm,测得的峰面积值与NDAOPPAM浓度在40.4～161.6mg·mL-1范围内呈线性关系,检出限(3S/N)为1ng.L-1。测得方法的日内和日间相对标准偏差(n=6)依次为0.53%和0.89%。在NDAOPPAM产品中残留的未反应完的反应物AAMAPN可用同样方法测定。测得从不同批号产品取得的3个样品中AAMPAN的质量分数分别为0.32%,0.43%,0.49%。Sample of N-{ 3-E 3-（ dimethylamino ）-l-oxo-2-propenyl ]-phenyl } acetamide （ abbreviated as NDAOPPAM） was dissolved and diluted to 100.0 mL with the mobile phase of mixture of methanol and H2O （38＋62）. Diamonsil C18 chromatographic column was used as stationary phase. Under the conditions described, NDAOPPAM was completed separated from 3-acetamidoacetophenenone （AAMAPN） which is one of the reactants in the synthesis of NDAOPPAM, and determined with ultraviolet detection at wavelength of 236 nm, Linear relationship between values of peak area and concentration of NDAOPPAM was obtained in the range of 40. 4-161.6 mg·L-1. Detection limit （3S/N） found was 1 ng ·L-1. Values of within-day and inter-day RSD＇s （n=6） found for NDAOPPAM were 0. 53%and 0. 89% respectively. The un-reacted reactant, AAMAPN, remained in the product NDAOPPAM was determined under the same way. Three samples taken from different batches were analyzed and contents of AAMAPN found were 0. 32%, 0. 43% and 0. 49% respectively.

关 键 词：反相高效液相色谱法 NDAOPPAM 相关物质 

分 类 号：O652.63[理学—分析化学]