Flurer C L
National Forensic Chemistry Center, US Food and Drug Administration, Cincinnati, OH 45202, USA.
J Pharm Biomed Anal. 1995 Jun;13(7):809-16. doi: 10.1016/0731-7085(95)01502-c.
The analyses of aminoglycoside antibiotics by capillary electrophoresis utilizing borate complexation and direct UV detection are discussed. Twelve aminoglycosides were studied and separated to demonstrate identification capabilities, with migration time RSDs from 0.21 to 0.44% (n = 6) for individual components. This buffer system permitted the detection of minor impurities such as precursors or closely related fermentation products. Quantification of dihydrostreptomycin and streptomycin was accomplished in 160 mM sodium tetraborate decahydrate with linearity over the range 0.050-1.0 mg ml-1. Determination of the purity of bulk dihydrostreptomycin was possible by the addition of the cationic surfactant myristyltrimethylammonium bromide. This reversed the electroosmotic flow, thereby reversing the migration order, and causing the streptomycin impurity to migrate before the dihydrostreptomycin main peak. Quantification was also demonstrated with the closely related compounds amikacin, bekanamycin, kanamycin A, and tobramycin, using sisomicin as an internal standard. The reproducibility of the method was typically 2-3% over 1 day, and 2% day-to-day. These studies illustrate the use of capillary electrophoresis for the identification and quantification of selected aminoglycosides as potential alternative methods to the assays given by the US Pharmacopeia.
本文讨论了利用硼酸盐络合和直接紫外检测通过毛细管电泳分析氨基糖苷类抗生素的方法。研究并分离了12种氨基糖苷类抗生素以展示其鉴别能力，各组分的迁移时间相对标准偏差（RSD）为0.21%至0.44%（n = 6）。该缓冲体系能够检测到诸如前体或密切相关的发酵产物等微量杂质。在160 mM十水合四硼酸钠中实现了二氢链霉素和链霉素的定量分析，线性范围为0.050 - 1.0 mg/ml。通过添加阳离子表面活性剂十四烷基三甲基溴化铵可以测定原料药二氢链霉素的纯度。这会使电渗流反转，从而使迁移顺序反转，导致链霉素杂质在二氢链霉素主峰之前迁移。以西索米星为内标，对密切相关的化合物阿米卡星、贝卡霉素、卡那霉素A和妥布霉素也进行了定量分析。该方法的重现性通常在1天内为2 - 3%，不同日期之间为2%。这些研究表明，毛细管电泳可用于选定氨基糖苷类抗生素的鉴别和定量分析，作为美国药典规定方法的潜在替代方法。
