摘要
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=0.997 8、0.998 5、0.999 2、0.998 9）;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。
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=0.9985）,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 were95.0%-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,accurate and reliable,and can be used for the determination of residual solvents in racemic ketoisoleucine calcium.
出处
《中国药房》
CAS
北大核心
2016年第21期2998-3000,共3页
China Pharmacy
作者简介
主管药师，硕士。研究方向：临床药学、药物制剂质量标准。电话：0731—84327455。E-mail：tangling82@126．com
通信作者：副主任药师，硕士。研究方向：药物制剂质量标准。电话：0731-84327265。E-maii：850326813@qq．com
