Daidone F, Heuvelmans R, Aerden L, Hoogmartens J, Adams E
Laboratory for Pharmaceutical Analysis, Faculteit Farmaceutische Wetenschappen, Katholieke Universiteit Leuven, O&N 2, Herestraat 49 (PB 923), B-3000 Leuven, Belgium.
J Pharm Biomed Anal. 2008 Sep 29;48(2):347-55. doi: 10.1016/j.jpba.2008.02.002. Epub 2008 Feb 12.
Out of three methods for the analysis of josamycin, the best one was selected and used as starting point for further development. A central composite design was applied to find the most influencing parameters and to optimize the chromatographic conditions and a full factorial design was used to perform a robustness study. The final method uses a Hypersil ODS column 5microm, 250mmx4.6mm i.d. maintained at 45 degrees C. The mobile phase is composed of acetonitrile-phosphate buffer (pH 3, 0.2moll(-1))-tetrabutylammonium hydrogen sulphate 0.2moll(-1)-water (21:5:3:71, v/v/v/v). Strongly retained impurities after the main peak require gradient elution, which is obtained by increasing linearly the acetonitrile concentration (from 21% to 50%, v/v) and decreasing the TBA concentration (from 3% to 0%, v/v) in the mobile phase. The total run time was 65min. UV detection is performed at 232nm and the flow rate is 1ml/min. The method shows good selectivity, precision, linearity and sensitivity. Five commercial bulk samples were analyzed.
在三种分析交沙霉素的方法中，选择了最佳方法并将其作为进一步开发的起点。应用中心复合设计来找出最具影响的参数并优化色谱条件，使用全因子设计进行稳健性研究。最终方法使用粒径为5微米、内径为250毫米×4.6毫米的Hypersil ODS柱，柱温保持在45℃。流动相由乙腈 - 磷酸盐缓冲液（pH 3，0.2mol/L） - 0.2mol/L硫酸氢四丁铵 - 水（21:5:3:71，v/v/v/v）组成。主峰之后的强保留杂质需要梯度洗脱，这通过在流动相中线性增加乙腈浓度（从21%至50%，v/v）并降低TBA浓度（从3%至0%，v/v）来实现。总运行时间为65分钟。在232nm处进行紫外检测，流速为1ml/min。该方法具有良好的选择性、精密度、线性和灵敏度。对五个市售原料药样品进行了分析。
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