HPLC-ECD法测定大观霉素的含量

Determination of Spectinomycin by HPLC-ECD

关键词:  HPLC-ECD  大观霉素  含量测定

Key words:  HPLC-ECD  Spectinomycin  Determination

摘要:

建立HPLC-ECD法测定大观霉素含量的分析方法。应用高效液相色谱—电化学检测器, Waters XBridge 色谱柱(C₁₈4.6mm i.d.?250,5μm),以pH3.2的草酸盐缓冲溶液—乙腈=1000：105为流动相,流速为1.0ml/min；柱后衍生溶液为21g/L的NaOH溶液,流速：0.5ml/min； ECD系统参数：Polarity:Positive； 检波： 0.12 volts,氧化电位： 0.70 volts,还原电位-0.60 volts,Range:5μA。结果表明，大观霉素及4R—二氢大观霉素在40μg/mL——320μg/mL范围内呈良好的线性关系(大观霉素r=0.9999,4R—二氢大观霉素r=0.9992),平均回收率为100.0%(n=9),RSD为0.2%。该方法有创新性,简便、准确,可用于大观霉素及相关制剂产品的质量控制。

Abstract:

Abstract： To establish the quantitative method for Spectinomycin by HPLC-ECD. The column used was a packed with 5?m Waters XBridge(C184.6mm i.d.?250，5μm).The mobil phase was a mixture of Ph3.2 Oxalate buffer and acetonitrile in aratio of 1000:105,with a flow rate of 1.0 ml/min; The Post-column derivatization solution was sodium hydroxide solution with the concentration 21g/L, with a flow rate of 0.5 ml/min.ECD System parameters : Polarity:Positive; Detector: 0.12 volts,Oxidation potential: 0.70 volts，Reduction potential:-0.60 volts，Range:5μA. The linear range of the Spectinomycin Dihydrochloride and (4R)-dihydrospectinomycin dihydrochloride was 40μg/mL—320μg/ml, the correlation coefficience of Spectinomycin Dihydrochloride was 0.9999，the correlation coefficience of (4R)-dihydrospectinomycin dihydrochloride was 0.9992. The average recovery rate was 100.0%（n=9）,RSD was 0.2%.The methed is innovative,reiable,simple precise,and be used for the quality control of Spectinomycin and Related finished products。