摘要
目的建立毛细管气相色谱法测定茴拉西坦中甲醇、乙醇、甲苯的残留量。方法采用INNO相键合聚乙二醇为固定液的毛细管石英色谱柱(30 m×0.53 mm,1.0μm);载气:氮气;以N,N-二甲基甲酰胺为溶剂;柱温:75℃,保持3 min,以15℃/min升温至150℃,保持5 min;进样口温度:200℃;检测器温度:200℃(FID)。结果甲醇在6.02～240.8 mg/L内线性关系良好,r=0.9998(n=5),定量限为1.97 mg/L,回收率为95.1%(RSD=2.9%);乙醇在12.07～251.5 mg/L内线性关系良好,r=0.9992(n=5),定量限为1.63 mg/L,回收率为100.6%(RSD=2.2%);甲苯在3.56～89.0 mg/L内线性关系良好,r =0.9999(n=5),定量限为0.59 mg/L,回收率为99.6%(RSD=1.1%)。结论本方法可用于茴拉西坦中甲醇、乙醇和甲苯的残留量测定。
Objective To develop a gas chromatographic method and determine the contents of residual organic solvents-methanol,ethanol and toluene in aniracetam. Methods Using a HP-INNOWAX capillary column and FID detector, N, N-dimethylformamide was used as the solvent. The oven temperature was set at 75 ℃ and maintained for 3 min, and the temperature was programmatically increased to 150 ℃ at the rate of 15 ℃ per min and maintained for 5 min. The temperature of injection port and the detector was set at 200 ℃. Resuits The linear range of methanol, ethanol and toluene were 6.02 - 240.8 mg/L, 12.07 - 251.5 mg/L and 3.56 - 89.0 mg/L, respectively,and the recovery rates were 95.1% （ RSD = 2.9% ） , 100.6% （ RSD = 2.2% ） and 99.6% （ RSD = 1.1% ）, respectively. The detection cimits of methanol, ethanol and toluene were 1.97,1.63 and 0.59 mg/L,respectively. Conclusion This method can be used to determine the residue level of methanol, ethanol and toluene in aniracetam.
出处
《现代食品与药品杂志》
2007年第3期34-36,共3页
JOurnal of Modern Food and Pharmaceuticals
