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目的:建立HPLC-ESI-IT-MSn方法,研究硫酸西索米星的杂质谱。方法:采用Agilent 1100 LC/MSD Trap液质联用仪,采用Gemini NX C18(4.6 mm×150 mm,5μm)色谱柱,以水-氨水-冰醋酸(96∶3.6∶0.4)为流动相A,甲醇为流动相B,梯度洗脱,流速1 mL.min-1;质谱检测器采用ESI离子源,正离子检测,离子源温度为350℃,雾化室压力为275.8 kPa,干燥气流速为9 L.min-1;检出杂质结构的鉴定方法根据有无杂质对照品而异:对于有对照品的杂质,通过比较其与对照品的色谱和质谱行为来确定结构;对于无对照品的未知杂质,则以已知结构物质如西索米星、奈替米星等为模型,通过分析已知物与未知杂质多级质谱行为的异同性推定其结构。结果:硫酸西索米星原料中检出16个有关物质,其中14个物质的结构得到归属。结论:本文建立的HPLC-ESI-IT-MSn方法及研究结果对硫酸西索米星的质量控制和工艺评价具有参考意义。
Objective: To establish HPLC-ESI-IT-MSn method to study impurity spectrum of sisomicin sulfate. Methods: An Agilent 1100 LC / MSD Trap LC / MS system was used with a Gemini NX C18 column (4.6 mm × 150 mm, 5 μm). The mobile phase A was eluted with aqueous ammonia-glacial acetic acid (96: 3.6: 0.4) Methanol as mobile phase B, gradient elution, flow rate 1 mL.min-1; MS detector using ESI ion source, positive ion detection, ion source temperature of 350 ℃, atomization chamber pressure of 275.8 kPa, dry gas flow rate of 9 L.min-1; Detection of impurity structure of the identification method depending on whether the impurity reference substance-specific: For impurities with reference substance by comparing its reference substance with the chromatographic and mass spectrometric behavior to determine the structure; For unknown substance is unknown Impurities, the structure of known substances such as sisomicin, netilmicin star as the model, by analyzing the similarities and differences between known and unknown impurities multi-level mass spectrometry to infer the structure. Results: Sixteen related substances were detected in the raw materials of sisomicin sulfate, and the structures of 14 substances were assigned. Conclusion: The HPLC-ESI-IT-MSn method and the results of this study have reference value for the quality control and process evaluation of sisomicin sulfate.