HS-GC法测定消旋酮异亮氨酸钙原料药中的4种残留溶剂

摘要

OBJECTIVE:To establish a method for the determination of 4 kinds of residual solvents in racemic ketoisoleucine calcium. METHODS:Headspace gas chromatography was performed on the column of DB-624 capillary column by temperature programmed,detector was FID,inlet temperature was 200 ℃,detector temperature was 250 ℃,carrier gas was nitrogen,flow rate was 1.0 ml/min,injection volume was 1 ml by headspace sampling,equilibrium temperature was 70 ℃ and equilibrium time was 30 min. RESULTS:The linear range was 120.04-480.16 μg/ml for methanol (r=0.997 8),200.21-800.83 μg/ml for ethanol (r=0.998 5),204.05-816.19 μg/ml for ethyl acetate(r=0.999 2),28.35-113.39 μg/ml for tetrahydrofuran(r=0.998 9);detection limits were 6.002 μg/ml,50.05 μg/ml,51.01 μg/ml and 7.087 μg/ml;RSD of precision was lower than 3%;recoveries were 95.0%-105.6%(RSD=3.95%,n=9),97.5%-106.4%(RSD=3.67%,n=9),98.1%-105.9%(RSD=3.16%,n=9)and 88.8%-99.2%(RSD=3.79%,n=9),respectively;4 kinds of residual solvents were not detected. CONCLUSIONS:The method is simple,accu-rate and reliable,and can be used for the determination of residual solvents in racemic ketoisoleucine calcium.%目的：建立测定消旋酮异亮氨酸钙原料药中4种有机溶剂残留量的方法。方法：采用顶空气相色谱法。色谱柱为DB-624毛细管柱，柱温采用程序升温，检测器为FID，进样口温度为200℃，检测器温度为250℃，载气为氮气，流速为1.0 ml/min，进样体积为1 ml，进样方式为顶空进样，顶空平衡温度为70℃，顶空平衡时间为30 min。结果：甲醇、乙醇、乙酸乙酯、四氢呋喃检测质量浓度线性范围分别为120.04～480.16、200.21～800.83、204.05～816.19、28.35～113.39μg/ml（r＝0.9978、0.9985、0.9992、0.9989）；检测限分别为6.002、50.05、51.01、7.087μg/ml；精密度试验的RSD＜3％；加样回收率分别为95.0％～105.6％、97.5％～106.4％、98.1％～105.9％、88.8％～99.2％，RSD分别为3.95％、3.67％、3.16％、3.79％（n＝9）；3批样品中4种残留溶剂均未检出。结论：该方法操作简单，结果准确、可靠，可用于消旋酮异亮氨酸钙原料药中的残留溶剂测定。