在线脱盐-高效液相色谱-离子阱-飞行时间质谱法鉴定盐酸多西环素有关物质结构

发布时间：2018-03-26 10:06

  本文选题：盐酸多西环素　切入点：在线脱盐-高效液相色谱-离子阱-飞行时间质谱法　出处：《中国药学杂志》2015年23期

【摘要】：目的应用在线脱盐-高效液相色谱-离子阱-飞行时间质谱(2D-LC-IT-TOF/MS)法鉴定盐酸多西环素片在药典条件下检出的有关物质结构,并推断盐酸多西环素在溶液状态下的降解途径。方法 LC 1 stD色谱条件:InertSustain~(TM)C_(18)(4.6 mm×150 mm,5μm)色谱柱,醋酸盐缓冲液[0.25 mol·L~(-1)醋酸-0.1 mol·L~(-1)EDTA钠盐-三乙胺(100:10:1),用醋酸或氨水调节pH值至8.8]-乙腈(85:15)为流动相进行等度洗脱;LC 2ndD色谱条件:InertSustain~(TM)C_(18)(2.1 mm×50 mm,2μm)色谱柱,0.1%甲酸冰溶液为流动相A,0.1%甲酸福乙睛为流动相B,进行梯度洗脱;质谱条件:ESI正负离子同时检测,雾化气流速1.5L·min~(-1),干燥气流速10 L·min~(-1)脱溶剂管温度200℃。根据多级质谱信息来推定药典条件下检出的有关物质结构和强制降解溶液中产生的杂质结构。结果在盐酸多西环素片中共检出8个有关物质推定出其中4个含量大于0.1%的有关物质的结构,分别为4-表多西环素、美他环素、β-多西环素、2-乙酰-6-脱碳酰胺多西环素。盐酸多西环素溶液在碱性条件下易降解,生成脱酮基开环物;在高温条件下容易产生4-表多西环素,并伴有少量4-表-6-表多西环素的生成;在酸性条件和光照条件下相对稳定。结论建立的方法可用于盐酸多西环素中杂质的鉴定,为盐酸多西环素的质量控制与工艺优化研究提供可靠的分析手段。
[Abstract]:Objective to identify the structures of related substances in doxycycline hydrochloride tablets under pharmacopoeia by on-line desalination, high performance liquid chromatography, ion trapping and time of flight mass spectrometry (TTOF / MS). The degradation pathway of doxycycline hydrochloride in solution was deduced. Methods the chromatographic conditions of LC 1 stD were as follows: 1. Acetic acid buffer solution [0.25 mol L~(-1)EDTA sodium salt-triethylamine 100: 10: 1, adjusted pH to 8.8 with acetic acid or ammonia] -acetonitrile: 8515) was used as mobile phase to perform isothermal elution with LC 2ndD chromatographic conditions:% InertCon sustained TMC182.1 mm 脳 50 mm ~ 2 渭 m) A 0.1% formic acid ice solution was used as mobile phase A0.1% formic acid as mobile phase. B was mobile phase B, gradient elution was carried out. Mass spectrometric conditions for simultaneous detection of positive and negative ions at 1: ESI level, The temperature of desolvent tube was 200 鈩，

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