反相高效液相色谱法测定硫酸西索米星氯化钠注射液的含量  

Determination of the content of sisomicin sulfate and sodium chloride injection by RP-HPLC

作　　者：侯玉荣 范青峰 史孙亮 袁耀佐 张玫 HOU Yurong;FAN Qingfeng;SHI Sunliang;YUAN Yaozuo;ZHANG Mei(Jiangsu Institute for Food and Drug Control,Nanjing 210019;China Pharmaceutical University,Nanjing 210009,China)

机构地区：[1]江苏省食品药品监督检验研究院,南京210008 [2]中国药科大学,南京210009

出　　处：《中国药科大学学报》2018年第6期695-698,共4页Journal of China Pharmaceutical University

基　　金：国家重大新药创制-化药制剂质量评价关键技术研究课题资助项目(No.2015ZX09303001)~~

摘　　要：建立硫酸西索米星氯化钠注射液含量测定的反相高效液相色谱法。色谱柱为Aminoglycoside RP 18 (4. 6 mm×150 mm,3μm),以庚烷磺酸钠溶液(取庚烷磺酸钠6 g,加0. 1 mol/L磷酸二氢钾溶液溶解并稀释至1 000 m L,用磷酸调节pH至1. 5)-乙腈(77∶23)为流动相,检测波长为205 nm,流速1. 0 m L/min,柱温35℃。西索米星峰与其相关物质及降解产物均分离良好。西索米星在0. 010 024～1. 002 4 mg/m L与峰面积呈良好的线性关系(Y=4. 210 2×10~6X+9. 107 0×10~3,r=0. 999 9,n=7),检出限0. 6 ng(相当于0. 000 1%),定量限2 ng(相当于0. 000 4%),回收率在99. 1%～100. 9%(RSD <1. 0%,n=9)。该方法简便灵敏、重复性好,能够用于硫酸西索米星氯化钠注射液的含量测定。较抗生素微生物检定法,专属性更好,缩小了结果的置信区间,节省检验时间。To establish a RP-HPLC method for the determination of content of sisomicin sulfate and sodium chloride injection.Thermo Aminoglycoside RP18(4.6mm×150mm,3μm)column was used.The mobile phase consisted of Sodium heptane sulfonate solution(take6g of sodium heptane sulfonate,add0.1mol/L potassium dihydrogen phosphate solution and dilute to1000mL,adjust the pH to1.5with phosphoric acid)-acetonitrile(77∶23).The detection wavelength was205nm,the flow rate was1.0mL/min.and the column temperature was35°C.The separation of sisomicin peaks with related substances and the degradation products was good.The linear range of the peak area with sisomicin was0.010024-1.0024mg/mL(Y=4.2102×10^6X+9.1070×10^3,r=0.9999,n=7),the detection limit was0.6ng,the limit of quantification was2ng,and the recovery rate was at99.1%-100.9%(RSD<1.0%,n=9).The method is sensitive,exclusive,accurate and suitable for the determination of sisomicin.Compared with the antibiotic microbiological test method,the specificity is better,the confidence interval of the result is narrowed,and the test time is saved.

关 键 词：反相高效液相色谱法 硫酸西索米星 质量标准 含量测定 

分 类 号：R917[医药卫生—药物分析学]