顶空气相色谱法测定异环磷酰胺中多种有机溶剂残留量  

Determination of Residual Organic Solvents in Ifosfamide by Headspace Gas Chromatography

作　　者：宋更申[1] 韩学静[1] 刘红莉[1] 

机构地区：[1]河北省药品检验所,河北石家庄050011

出　　处：《中国药业》2009年第23期21-22,共2页China Pharmaceuticals

摘　　要：目的建立分离测定异环磷酰胺原料中残留的多种有机溶剂的方法。方法采用顶空气相色谱法,色谱柱为H P-INNOW ax毛细管柱,载气为氮气,FID检测器,柱温采用程序升温,外标法测定异环磷酰胺中乙醚、丙酮、四氢呋喃、二氯甲烷、甲醇、乙醇的残留量。结果6种有机溶剂能完全分离,质量浓度在所考察的范围内与峰面积线性关系良好,r为0.9996～1.0000,平均回收率为94.6%～100.5%,精密度的RSD均不大于10%,检测限为20～2350ng/mL。结论顶空气相色谱法快速、灵敏、准确,适用于异环磷酰胺中多种有机溶剂残留量的测定。Objective To establish a method for the determination of six residual organic solvents in ifosfamide raw material. Methods The residual solvents in ifosfamide such as ethyl ether, propanone, tetrahydrofuran, dichloromethane, methanol, ethanol, were quantitatively determined by headspace gas chromatography （GC） on HP-INNOWax column, with FID detector, nitrogen as the carries, Results Six residual solvents were completely separated. There was the good linearity （ r = 0. 999 6 - 1. 000 0）. RSD of precision was less than 10%. The average recovery rate was in the range of 94.6%- 100. 5%. The detection limits was between 20-2 350 ng/mL. Conclusion The method is rapid, sensitive and accurate, which can be used for the determination of residual organic solvents in ifosfamide.

关 键 词：异环磷酰胺 有机溶剂残留量 顶空气相色谱法 

分 类 号：R927.11[医药卫生—药学] R979.1