摘要
目的建立克林霉素磷酸酯原料药中三乙胺残留量的测定方法。方法顶空进样毛细管气相色谱法,采用Elite-5Amine(5%二苯基-95%二甲基聚硅氧烷固定液)石英毛细管柱,柱温50℃,溶解介质为1.0mo1/L NaOH溶液,载气为氮气,检测器为FID,测定三乙胺的残留量。结果在上述色谱条件下三乙胺峰形最佳,峰面积与浓度呈良好的线性关系(r=0.9999),精密度和回收率良好,定量限为0.0466?g/mL,检测限为0.0155?g/mL。结论本法简单、灵敏、准确,适用于克林霉素磷酸酯中三乙胺残留量的测定。
Objective To establish a method for determination of residual triethylamine in clindamycin phosphate. Methods It was quantitatively determined by headspace gas chromatography on Elite-5Amine (5%diphenyl-95%dimethyl polysiloxane) capillary column with FID detector, nitrogen as the carries. The column temperature was 50℃, the sample was dissolved in 1.0mol/L NaOH solution. Results The peak shape of triethylamine is quite well. The calibration curve of triethylamine shows a good linearity with precision and accuracy (r=0.9999). The limit of quantification is 0.0466μg/mL, the detection limit is 0.0155μg/mL. Conclusion This method appears to be simple, sensitive and accurate. It can be used for determining the content of residual triethylamine in clindamycin phosphate.
出处
《中国抗生素杂志》
CAS
CSCD
北大核心
2014年第3期217-219,共3页
Chinese Journal of Antibiotics