RP-HPLC法测定N-[3-[3-(二甲基氨基)-1-氧基-2-丙烯基]-苯基]-乙酰胺的含量及其有关物质

RP-HPLC determination of content of N-[3-[3-(dimethylamino)-1-oxo-2-propenyl]-phenyl]-lacetamide and its related substances

目的:采用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]-乙酰胺含量及其有关物质。方法:采用DiamonsilTM(钻石)C18(250 mm×4.6 mm,5μm)色谱柱,流动相为甲醇-乙腈-水(2∶21∶77)流速1.0mL.min-1,检测波长238 nm。结果:在本文色谱条件下N-[3-[3-(二甲基氨基)-1-氧基-2-丙烯基]-苯基]-乙酰胺与有关物质能达到有效分离,在52.84～211.36μg.mL-1范围内线性关系良好,r=0.9998;仪器精密度RSD为0.95%;方法重复性RSD为1.2%;最低检测限3.18 ng。结论:该方法简便、准确、可行,可用于N-[3-[3-(二甲基氨基)-1-氧基-2-丙烯基]-苯基]-乙酰胺的质量控制。

Objective： A reversed phase high performance liquid chromatography method for the determination of content of N - [ 3 - [ 3 - （dimethylamino） - 1 - oxo - 2 - propenyl ] - phenyl ] - lacetamide and its related sub- stances. Methods： The analysis was performed on Diamonsil C18 reversed - phase analytical column（250 mm ×4. 6 mm,5 μm）;the mobile phase consisted of a mixture of methanol- acetonitrile- water（2： 21： 77）at the flow rate was 1.0 mL · min ^-1; The ultraviolet detection wavelength was set at 238 nm. Results：N- [3 - [3 - （dimethylamino） - 1 - oxo - 2 - propenyl] phenyl ] - aeetamide and its related substances could be seperated well. The linearity of the N - [ 3 - [ 3 - （dimethylamino） - 1 - oxo - 2 - propenyl - phenyl ] - acetamide curve was well correlated （ r = 0. 9998） within the range of 52. 84 -211.36 μg ·mL^- 1. The instrument precision RSD was 0. 95% ;The method precision RSD was 1.2% ;The detection limit was 3. 18 ng. Condusion：The method appeared to be simple, accurate and reproducible; h can be used to control the quality of N- [ 3 -[ 3 -（dimethylamino） -1 -oxo- 2- propenyl ] -phenyl ]-acetamide.