气相色谱法测定米力农中残留溶剂

目的建立气相色谱法测定米力农中的残留溶剂。方法采用气相色谱法,FID检测器,在毛细管柱DB-624(30m×0.53 mm,3μm)上程序升温,载气为氮气,进样口温度200℃,检测器温度200℃,以二甲基亚砜为溶剂配制对照溶液及供试品溶液。结果四种有机溶剂完全分离,在所考察的浓度范围内具有良好的线性,甲醇、乙醇、二氯甲烷、乙酸的检测限分别为3.56、4.05、1.19、1.05μg.mL-1,精密度RSD均小于3.5%。平均回收率为98.8%、99.5%、100.6%、101.5%。结论经方法学验证,本方法简便灵敏,结果准确可靠,适用于米力农原料药中残留溶剂的检测。

Determination of residual solvents in Milrinone by GC

OBJECTIVE To establish a method for determining the residues of four kinds of solvents in Milrinone by gas chromatography.METHODS The detector was FID.The analytical column was DB-624(30m×0.53mm,3μm).The injector temperature was 200℃,and the detector temperature was 200℃.The column temperature was programmed raised.Nitrogen as the carrier gas and the dimethylsulfoxide(DMSO) as solvent media.RESULTS It appeared a good linearity in the experimental concentration.The detector limit of methanol,ethanol,dichloromethane,acetic acid separately was 3.56,4.05,1.19 and 1.05μg·mL-1respectively.The RSD of precision were all less than 3.5%.The average recovery was 98.8%,99.5%,100.6% and 101.5% respectively.CONCLUSION This method was simple,sensitive,accurate,and can be used for detection of four residual solvents in Milrinone.