高效液相色谱-蒸发光散射检测法测定盐酸大观霉素的含量

Content determination of spectinomycin hydrochloride by HPLC with ELSD

目的 :应用高效液相色谱 -蒸发光散射检测 (HPL C/ EL SD)法分析盐酸大观霉素含量。方法 :采用 Diamonsl TM(钻石 ) C1 8色谱柱 (2 5 0 mm× 4 .6 mm,5μm) ;流动相 :0 .0 2 mol/ L三氟醋酸水溶液 -乙腈 (99:1) ;检测器条件 ,漂移管温度为 5 0℃ ,雾化气体 (空气 )压力为 3.0 bar。结果 :盐酸大观霉素在 2 .72 5～ 10 .90 4μg范围内 ,进样量对数值与峰面积对数值呈良好的线性关系 ;理论板数以大观霉素峰计算为 5 10 0。结论 :本方法操作简单 ,准确性、重现性好 ,与微生物效价法比较 ,测定大观霉素含量无显著性差异 ,可用于盐酸大观霉素成品的质量控制。

Object:To establish an HPLC/ELSD method for the content analysis of spectinomycin hydrochloride. Methods: The separation was performed on a Diamonsil C18 column (150 mm×4.6 mm,5 μm).The mobile phase consists of 0.02 mol/L TFA-acetonitrile(99∶1,v/v).The temperature of the drift tube was set at 50oC, and the gas pressure was 3.0 bar. Results: In the range of 2.725～10.904 μg, there was a good linear relationship between the log value of the inject quantities and the log value of the peak areas. The number of theoretical plates calculated on spectinomycin peak was 5100. Conclusion:The method was simple, accurate and highly reproducible. There was no significant difference between the HPLC/ELSD and biological method in content analysis of the sample. This method is suitable for quality control of spectinomycin hydrochloride.