二维高效凝胶色谱反相液相色谱-质谱联用技术分析注射用阿洛西林钠中的聚合物杂质

发布时间：2018-03-21 10:06

本文选题：注射用阿洛西林钠　切入点：聚合物杂质　出处：《中国药学杂志》2017年14期 　论文类型：期刊论文

【摘要】：目的对注射用阿洛西林钠中的聚合物杂质进行分离定位及结构鉴定,并对高效凝胶色谱法测定其聚合物杂质的有效性进行考察。方法利用二维液相色谱-质谱联用技术对注射用阿洛西林钠中的聚合物杂质进行分离定位及结构鉴定。一维高效凝胶色谱以Ultimate SEC-120为色谱柱,以p H 7.0的5 mmol·L~(-1)磷酸盐缓冲液等度洗脱;二维以XBridge C18为色谱柱,以10 mmol·L~(-1)甲酸铵溶液(p H 6.5)和8 mmol·L~(-1)甲酸铵的乙腈-水(200∶50)溶液梯度洗脱。以质谱仪作为检测器对其进行检测,并进行结构鉴定。结果高效凝胶色谱法测定注射用阿洛西林钠的聚合物杂质色谱峰除聚合物杂质外,还包括阿洛西林青霉烯酸及阿洛西林青霉烯酸脱羧产物。反相液相色谱系统中定位出4种聚合物杂质,并推断出其可能的化学结构。结论二维液相色谱-质谱联用技术可有效分离、定位并鉴定注射用阿洛西林钠中的聚合物杂质,为有效控制β-内酰胺抗生素中的聚合物杂质提供了新思路。
[Abstract]:Objective to separate, locate and identify the polymer impurities in aloxicillin sodium for injection. The effectiveness of high performance gel chromatography for the determination of polymer impurities was investigated. Methods the polymer impurities in aloxicillin sodium for injection were separated, located and identified by two-dimensional liquid chromatography-mass spectrometry. 1 D high performance gel chromatography was performed on Ultimate SEC-120 column. It was eluted with 5 mmol 路L ~ (-1) phosphate buffer of pH 7.0, with XBridge C _ (18) column, with 10 mmol 路L ~ (-1) ammonium formate solution (pH 6.5) and 8 mmol 路L ~ (-1) ammonium formate with gradient elution in acetonitrile-water (200 ~ (50)) solution. It was determined by mass spectrometer. Results the polymer impurity chromatographic peak of aloxicillin sodium for injection was determined by high performance gel chromatography except polymer impurity. It also includes aloxicillin penicillenoic acid and aloxicillin penicillinic acid decarboxylation products. Conclusion Two-dimensional liquid chromatography-mass spectrometry can effectively separate locate and identify the polymer impurities in aloxicillin sodium for injection. It provides a new idea for the effective control of polymer impurities in 尾-lactam antibiotics.
【作者单位】：浙江省食品药品检验研究院;浙江工业大学;
【基金】：2015年浙江省公益技术研究社会发展项目资助(2015C33168)
【分类号】：O657.63;R927.1

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