摘要
2,4,6 -三硝基苯磺酸做衍生试剂 ,采用反相高效液相色谱法分析、紫外检测器检测 ,分离、定量了硫酸阿米卡星注射液及有关杂质 A、B、C、D。本法的衍生化产物稳定 ,线性范围为 0 .2～ 2 0 mg/ ml(r=0 .9991) ,平均回收率为 (10 0 .4± 2 .0 ) % ,日内、日间、不同人之间的操作误差分别为 1.2 9%、0 .90 %、0 .6 0 % ,最低检出量为 0 .0 5 6 ng。用本法测定了国内 2 1个厂家 2 4批硫酸阿米卡星注射液的含量 ,并与微生物法结果比较 ,用自身配对 t检验法考察两法结果差异。结果表明 ,绝大多数厂家的产品采用两法测定结果一致 (n=2 2 ) ,但也有个别厂家的产品 ,采用微生物法测定结果明显比本法高 ,其高效液相色谱图显示该类产品中杂质A的含量较高。不同厂家的产品中的杂质种类、含量也有较大差异 ,国产硫酸阿米卡星注射液中最常见的杂质是杂质
The analysis of commercial amkacin sulfate injection from different origins by reverse phase high performance liquid chromatography (RP HPLC) on a Diamonsil C 18 column with UV detection (340nm) was described. The mobile phase consists of 75 volumes of methanol and 25 volumes of a 0.27% solution of potassium dihydrogen phosphate, pH6.5. Samples were derivatized with 2,4,6 trinitrobenzenesulfonic acid. The derivatized products are stable within 8 hours at ambient temperature. The linear ranges were 0.2~20mg/ml ( r =0.9991); mean recovery: (100.4±2.0)%; inter day, intra day relative standard deviations were 0.90% and 1.29%, respectively; the detection limit was 0.056ng. 24 batches of amikacin sulfate injection were determined with this method and microbial assay, respectively. The differences between both methods were negligible for most samples, but in some cases, the results obtained with microbial assay were higher than that of HPLC. The chromatography profile showed there was a kind of antibacterial impurity presenting a large percentage in these special samples, demonstrating the reason of the above differences.
出处
《中国抗生素杂志》
CAS
CSCD
北大核心
2001年第5期345-347,392,共4页
Chinese Journal of Antibiotics
