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目的:建立测定替卡西林钠克拉维酸钾(15∶1)中高分子杂质的HPLC分析方法。方法:采用高效液相色谱法,以TSKG2500 PWXL(7.8 mm×300 mm,7μm)为色谱柱,以pH 8.0磷酸盐缓冲液[0.15 mol.L-1磷酸氢二钠溶液-0.15 mol.L-1磷酸二氢钠溶液(95∶5)]为流动相,流速0.8 mL.min-1,检测波长230 nm,柱温30℃。结果:高分子杂质与替卡西林及克拉维酸能较好分离;替卡西林的检测限为4.0 ng,克拉维酸的检测限为3.7 ng;替卡西林线性范围为0.052~0.32μg(r=0.9999),高分子杂质在进样量以替卡西林计为11.2~30.3μg范围内时,与峰面积线性关系良好(r=0.9992);重复性较好(RSD=0.52%,n=5)。结论:该方法简单、快速、准确,重复性好,可用于替卡西林钠克拉维酸钾(15∶1)中的高分子杂质检测。
OBJECTIVE: To establish an HPLC method for the determination of high molecular impurities in tacrolimin sodium clavulanate potassium (15: 1). METHODS: High performance liquid chromatography (HPLC) was performed on a TSKG2500 PWXL (7.8 mm × 300 mm, 7 μm) column with pH 8.0 phosphate buffer [0.15 mol·L -1 disodium hydrogen phosphate solution-0.15 mol·L- 1 sodium dihydrogen phosphate solution (95: 5)] as the mobile phase at a flow rate of 0.8 mL.min-1. The detection wavelength was 230 nm and the column temperature was 30 ℃. Results: The detection limit of ticarcillin was 4.0 ng, the detection limit of clavulanic acid was 3.7 ng, the linear range of ticarcillin was 0.052-0.32 μg (r = 0.9999). When the amount of polymer was measured in the range of 11.2-30.3 μg for ticarcillin, the linear relationship was good (r = 0.9992); the repeatability was better (RSD = 0.52%, n = 5 ). Conclusion: The method is simple, rapid, accurate and reproducible. It can be used to detect the impurity of tacrolimus potassium clavulanate (15:1).