论文部分内容阅读
目的建立反相高效液相色谱(RP-HPLC)法测定注射用替加环素的有关物质。方法采用Phenomenex Gemini C_(18)柱(4.6 mm×150 mm,3μm);以20 mmol·L~(-1)磷酸氢二钾和2.5 mmol·L~(-1)乙二胺四乙酸二钠溶液(用磷酸调节pH值至6.4)为流动相A;以乙腈为流动相B;以1.0 mL·min~(-1)的流速进行梯度洗脱;检测波长为248 nm;柱温为30℃。结果在该色谱条件下,替加环素与各杂质分离良好,主峰纯度大于998,物料基本平衡。以替加环素校正因子为1,米诺环素、9-氨基米诺环素、9-硝基米诺环素、Di-Ma-Tig、CMI校正因子分别为1.17、0.94、1.36、1.05、1.03。结论所建立的RP-HPLC法能准确测定注射用替加环素的有关物质,可用于注射用替加环素的质量控制。
Objective To establish a reversed-phase high performance liquid chromatography (RP-HPLC) method for the determination of related substances of tigecycline for injection. Methods Phenomenex Gemini C_ (18) column (4.6 mm × 150 mm, 3 μm) was used. With 20 mmol·L -1 dipotassium phosphate and 2.5 mmol·L -1 disodium ethylenediaminetetraacetate The solution was adjusted to pH 6.4 with phosphoric acid as mobile phase A; acetonitrile was used as mobile phase B; gradient elution was performed at a flow rate of 1.0 mL · min -1; the detection wavelength was 248 nm; the column temperature was 30 ℃ . Results Under the chromatographic conditions, tigecycline was well separated from the impurities, the main peak purity was greater than 998, the material was basically balanced. The calibration curve of tioguancinc was 1, minocycline, 9-aminominocycline, 9-nitrominocycline, Di-Ma-Tig and CMI were 1.17, 0.94, 1.36, , 1.03. Conclusion The established RP-HPLC method can accurately determine the relevant substances of tigecycline for injection and can be used for the quality control of tigecycline for injection.