顶空气相色谱法测定美罗培南原料残留有机溶剂

Determination of Residual Organic Solvents of Meropenem Crude Drug by Headspace GC

目的:建立美罗培南原料药中丙酮、乙睛、二氯甲烷、四氢呋喃和乙酸乙酯有机溶剂残留量的顶空气相色谱测定法。方法:色谱条件:FID检测器,DB-624石英毛细管柱(30 m×0.321 mm×1.80μm),柱温50℃。结果:丙酮、乙睛、二氯甲烷、四氢呋喃、乙酸乙酯分别在0.025～139.600、0.053～70.700、0.012～39.800、0.016～70.100、0.039～43.000 mg·ml^(-1)的浓度范围内线性关系良好(r>0.999 0);丙酮、乙睛、二氯甲烷、四氢呋喃、乙酸乙酯的回收率分别为:97.7%、96.7%、98.3%、95.4%、96.6%,RSD均小于5.0%。结论:本方法简便、准确、重复性好,可在同一色谱系统中测定美罗培南原料生产过程中残留的5种有机溶剂。

Objective： To develope a method using GC coupled with FID and headspace for the determination of residual organic solvents （ acetone, acetonitrile, dichlormethane, tetrahydrofuran, and acetoacetate） of meropenem crude drug. Method： The residual organic solvents in meropenem crude drug were determined by headspace GC on DB-624 capillary column（30 m ×0. 321 mm × 1. 80μm） with FID and the column temperature was 50 ℃. Result： The method was sensitive with good linearity （r 〉0. 999 0） over the range of 0. 025-139. 600 mg· ml^-1 for acetone, 0. 053-70. 700 mg· ml^-1 for acetonitrile, 0. 012-39. 800 mg· ml^-1 for dichlormethane, 0. 016- 70. 100 mg· ml^-1 for tetrahydrofuran and 0. 039-43.000 mg· ml^-1 for acetoacetate. The recovery of acetone, acetonitrile, dichlormethane,tetrahydrofuran, acetoacetate were 97. 7% ,96. 7% ,98. 3% ,95.4% ,96.6% respectively, and RSD of all were less than 5.0%. Conclusion： The method is simple, accurate, and reproducible, which can be applied to determine residual organic solvents of meropenem crude drug.