顶空毛细管气相色谱法测定美司钠原料和注射液的残留溶剂  

Determination of residual solvents in mesna crude material and injection by headspace capillary gas chromatography

作　　者：张秉华 王小亮 郭欢迎 马丽 ZHANG Binghua;WANG Xiaoliang;GUO Huanying;MA Li(Shaanxi Institute for Food and Drug Control,Xi′an 710065,China;Department of Pharmacy,the Central Hospital of Xianyang,Xianyang 712000,China)

机构地区：[1]陕西省食品药品监督检验研究院,西安710065 [2]咸阳市中心医院药学部,咸阳712000

出　　处：《西北药学杂志》2019年第1期39-43,共5页Northwest Pharmaceutical Journal

摘　　要：目的建立美司钠原料及其注射剂中4种残留溶剂的顶空毛细管气相色谱测定方法。方法使用HP-1毛细管气相色谱柱(30m×0.25mm,0.25μm),采用程序升温。初始温度为40℃,保持5min,再以20℃·min-1升温至150℃;进样口温度为200℃;检测器为FID;检测器温度为250℃。顶空进样,平衡温度为75℃,平衡时间为30min。结果同时测定了美司钠原料和注射液中4种残留有机溶剂,甲醇、乙醇、异丙醇和丙酮分离度均在2.0以上,线性范围分别为6.6～66.0(r1=0.999 4),4.9～49.1(r2=0.999 9),5.8～58.0(r3=0.999 5)和8.0～80.0μg·mL-1(r4=0.999 6),平均加样回收率分别为97.3%,98.2%,99.5%和99.1%,RSD值分别为1.9%,2.1%,1.5%和1.7%。结论该方法灵敏、准确,可用于美司钠原料及其注射液中残留溶剂的检测。Objective To establish a headspace capillary gas chromatography method for the determination of 4 residual solvents in mesna crude material and injection.Methods The determination was performed on an HP-1 column(30 m×0.25 mm,0.25μm)with the initial temperature at 40℃maintaining for 5 min,and then up to 150℃with a speed of 20℃·min-1 through temperature-programmed route.The inlet temperature was 200℃and the FID was used as a detector which was set at 250℃.Headspace sampling was used with temperature of equilibrium at 75℃and the equilibrium time 30 min.Results 4 kinds of organic solvents in mesna crude material and injection were determined simultaneously.The resolution between methanol,ethanol,isopropanol and acetone were all above 2.0 and the calibration curves were all with good linearity in the ranges of 6.6-66.0μg·mL^-1 for methanol(r1=0.999 4),4.9-49.1μg·mL^-1 for ethanol(r2=0.999 9),5.8-58.0μg·mL^-1 for isopropanol(r3=0.999 5)and 8.0-80.0μg·mL^-1 for acetone(r4=0.999 6).The average recoveries were 97.3%,98.2%,99.5%and 99.1%with RSD 1.9%,2.1%,1.5%and 1.7%,respectively.Conclusion The method was proved to be accurate,sensitive,and can be used for the detection of residual solvents in crude material and injection.

关 键 词：美司钠 顶空气相色谱法 残留溶剂 

分 类 号：R917[医药卫生—药物分析学]