摘要
目的采用顶空毛细管气相色谱法(HSp-CGC)测定热不稳定铵盐化合物XY03中的游离正丁胺。方法色谱柱为SE-54(50 m×0.25μm,1μm)石英毛细管柱,载气为N2(3 mL.min-1)、H2(42 mL.min-1)、空气(80 mL.min-1),检测器为FID,柱温120℃,进样温度200℃,检测温度200℃,顶空温度40℃,平衡时间90 min,进样气体1 mL。结果 1.0～10 mg.mL-1正丁胺与峰高的线性关系良好,回归方程为:Y=11.982X-9.029×103(r=0.9991),检测限为2.5 ng.mL-1(S/N≥3),定量限为10 ng.mL-1(S/N≥10);进样精密度、重复性、中间精密度(RSD)分别为2.84%、2.57%、2.35%,平均回收率为101.2%(RSD=2.07%)。3批XY03铵盐产品中游离正丁胺的含量分别为1.74%、1.73%、1.63%。结论 HSp-CGC法可选择性地将热不稳定铵盐XY03中的游离正丁胺汽化并测定,所用方法快速、简便、准确,是检测铵盐类化合物中游离胺的一种较实用的方法。
OBJECTIVE To study free n-butylamine of thermally unstable ammonium salt XY03 by headspace capillary gas chromatography（HSp-CGC）.METHODS SE-54（50 m× 0.25 μm,1μm）silica capillary column was selected and the flow rate of carrier gase was 3 mL·min-1（N2）,42 mL·min-1（H2） and 80 mL·min-1（air）.The detector was FID.The column temperature was 120℃.The injection temperature was 200 ℃ and the detection temperature was 200 ℃.The temperature of headspace was 40 ℃ with 90 minutes＇ equilibration.The gas injection volume was 1 mL.RESULTS The linear equation of n-butylamine concentration was Y=11.982X-9.029×103（r=0.9991）.The limit of detection was 2.5 ng·mL-1（S/N≥3） and the limit of quantification was 10 ng·mL-1（S/N≥10）.The injection precision,repeatability and intermediate precision（RSD）were 2.84%,2.57% and 2.35%,respectively.The average recovery was 101.2%（RSD=2.07%）.The content of free n-butylamine in three batches of XY03 ammonium were 1.74%,1.73% and 1.63%,respectively.CONCLUSION HSp-CGC could selectively evaporate the free n-butylamine of XY03 and determine it quantitatively.It is a rapid,simple and accurate method which could be used in quantitative determination of the free amine in ammonium compounds.
出处
《华西药学杂志》
CAS
CSCD
北大核心
2012年第6期694-696,共3页
West China Journal of Pharmaceutical Sciences
