气相色谱法测定泊马度胺中5种残留溶剂

Determination of Five Kinds of Residual Solvents in Pomalidomide by Gas Chromatography

目的:建立气相色谱法测定泊马度胺中甲醇、乙醇、乙酸乙酯、二氧六环与乙酸残留量的方法。方法:采用以6%氰丙基苯基-94%二甲基聚硅氧烷(或极性相近)为固定液的毛细管柱,FID检测器,以氮气为载气,二甲基亚砜为溶剂,直接进样。结果:在选定的色谱条件下,各成分可达到很好的分离;甲醇、乙醇、乙酸乙酯、二氧六环与乙酸分别在76.28~610.20、126.38~1011.00、127.53~1020.20、10.30~82.40、126.5~1012.40μg·mL-1的范围内线性良好(r=0.9950~0.9999);精密度、重复性的RSD均不大于10.0%;回收率分别为100.9%、97.95%、100.0%、98.79%、98.90%(n=9,RSD<10%)。甲醇、乙醇、乙酸乙酯、二氧六环与乙酸的检测限分别为0.60、0.80、0.80、1.55、2.02μg·mL-1;定量限分别为1.51、2.00、2.01、3.87、5.04μg·mL-1。测定供试品3批,甲醇检出量分别为0.015%、0.014%、0.013%;乙醇检出量分别为0.145%、0.212%、0.124%;乙酸乙酯、二氧六环、乙酸均未检出。结论:该方法简单准确,灵敏度高,专属性强,适于测定泊马度胺中甲醇、乙醇、乙酸乙酯、二氧六环与乙酸等5种残留溶剂的残留量。

Objective:To establish a gas chromatography(GC)method for determination of methanol,ethanol,ethyl acetate,1,4-dioxane and acetic acid in pomalidomide. Methods:A capillary column with 6% cyanpropyl phenyl-94% dimethyl siloxane(or similar polarity)as stationary phase was adopted. The test was performed with FID detector,DMSO solvent,and nitrogen as the carrier gas and direct injection. Results:Each component could be separated well under the chromatographic condition. There were good linear relationship with r=0.9950~0.9999 in the range of 76.28~610.20,126.38~1011.00,127.53~1020.20,10.30~82.40 and 126.5~1012.40 μg·mL-1 for methanol,ethanol,ethyl acetate,1,4-dioxane and acetic acid respectively. The RSDs of the precision and repeatability were not more than 10.0%. The recoveries were 100.9%,97.95%,100.0%,98.79% and 98.90% for methanol,ethanol,ethyl acetate,1,4-dioxane and acetic acid respectively(n=9,RSD<10%). The limits of quantitation of methanol,ethanol,ethyl acetate,1,4-dioxane and acetic acid were 0.60,0.80,0.80,1.55,2.02 μg.mL-1 respectively. The limits of detection of methanol,ethanol,ethyl acetate,1,4-Dioxane and acetic acid were 1.51,2.00,2.01,3.87,5.04 μg·mL-1 respectively. Three batches of samples were tested,the detectable amount of methanol was 0.015%,0.014% and 0.013%,ethanol was 0.145%,0.212% and 0.124%,ethyl acetate,1,4-dioxane and acetic acid were not detected. Conclusion:The method is simple and accurate with high sensitivity and good specificity. It can be applicable to the determination of 6 residual solvents in pomalidomide.