气相色谱法检查依托咪酯注射液中二甘醇的含量

Determination of Diethylene glycol in Etomidate Injection by GC

目的建立依托咪酯注射液中二甘醇检查方法。方法采用气相色谱法,以丙三醇为内标,色谱柱为INNOWAX毛细管柱（30m×0.53mm×1μm）,汽化室温度220℃,程序升温：初始温度为120℃,保持3分钟;以每分钟10℃的速度升至230℃,保持5min。载气：氮气,4mL·min^-1;检测室温度250℃,尾吹30mL·min^-1,进样量1μL。结果上述测定方法能使内标（丙三醇）、1,2-丙二醇、1,3-丙二醇和二甘醇良好分离,在11μg·mL^-1-167μg·mL^-1的范围内浓度（C）与峰面积响应值（f=A/A内）有良好的线性关系,r=0.9995;进样精密度、日内测定精密度、日间测定精密度的RSD%分别为1.1%、0.9%和1.0%;平均回收率（n=9）为100.9%,RSD为1.5%;方法定量限和检测限分别为0.56μg·mL^-1,0.17μg·mL^-1。结论气相色谱法可以用于检查控制依托咪酯注射液中二甘醇的含量。

OBJECTIVE To determine Diethylene glycol in Etomidate Injection by GC.METHODS GC was applied to quantitative analysis.Chromatographic conditions were： INNOWAX column（30m×0.53mm×1μm）;Flame ionization detector（FID）;Column temperature： Maintaining the temperature of column at 120℃ for 3 minutes,then raising the temperature at a rate of 10℃ per miniutes to 230℃ for 5 minutes;Injector temperature： 220℃;Detector temperature： 240℃;Nitrogen was used as carrier gas,the flow rate was 4 mL·min^-1.An internal standard was glycerol.RESULTS The calibration curve was linear in the range of 11μg·mL^-1～167μg·mL^-1.The average recoveries（n=9） was 100.9%.CONCLUSION The established method is accuracy,sensitive and simple.