喹诺酮药物光稳定性实验HPLC分析方法的建立

The establishment of HPLC method for monitoring of photostability of quinolone antibiotics

目的:建立适用于多种喹诺酮药物光稳定性试验的通用 HPLC 方法。方法:采用 YMC ODS-AM,5μm,4.6 mm×150mm 色谱柱,流动相为0.07%三氟醋酸溶液(三乙胺调 pH 至2.5±0.1)-乙腈(根据分析的品种调整乙腈比例为14%～22%),柱温为40℃;流速为1 mL·min^(-1);DAD 检测波长范围为200～400 nm。结果:二极管阵列检测器(PDA)及低分辨质谱检测显示方法的专属性良好;最大日内及日间误差(RSD)均小于1%,重复性(RSD)约1%;最低检测限约1 ng;线性范围为0.07～15μg。结论:本方法不仅可用于洛美沙星、莫西沙星、加替沙星、格帕沙星、环丙沙星的光稳定性试验,其流动相系统还适用于 LC/MS 分析。

Objective：An HPLC method with good applicability in monitoring photodegradation of quinolone drugs was developed. Methods：A YMC ODS- AM column（5 μm,4.6 mm × 150 mm） was used, and the mobile phase was a mixture of 0. 07% trifluoro acetic acid （adjust to pH 2. 4 ± 0. 1 with triethylamine） -acetonitrile, according to the samples the proportion of acetonitrile was adjusted from 14% to 22% appropriately. The temperature for separation was 40 ℃. A photo - diod array detector was used with wavelength in the range of 200 to 400 nm. Result： The method shows good specificity, and good reproductivity with RSDmax not more than 1%. Limit of detection was 1 ng. The linearity range from 15 μg to 0. 07 μg. Conclusion：The method is suitable for the photostability experiment of lomefloxacin, moxifloxacin, gatifloxacin, grepafloxacin and ciproiloxacin ; and its mobile phase is suitable for LC/MS.