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...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。展开更多
A two-dimensional LC(2D-LC)method was coupled to an ion mobility-high-resolution mass spectrometer(IM-MS),which enables the separation of complex samples in four dimensions[2D-LC,ion mobility(IM)and mass spectrometry(...A two-dimensional LC(2D-LC)method was coupled to an ion mobility-high-resolution mass spectrometer(IM-MS),which enables the separation of complex samples in four dimensions[2D-LC,ion mobility(IM)and mass spectrometry(MS)].This approach works as a continuous multiheart-cutting LC-system,using a long modulation time of four minutes,in comparison to comprehensive two-dimensional liquid chromatography,which allows the complete transfer of most of the first dimension peaks to the second dimension column without fractionation.Hence,each compound delivers only one peak in the second dimension,which simplifies the data handling even when ion mobility as a third and mass spectrometry as a fourth dimension are introduced.The analysis of different complex samples,such as a plant extract from Hediotys diffusa and Scutellaria barbata,a waste water inflow,and a biocoal sample,was shown.The results of the four-dimensional separation method demonstrate that with the same column combination and the same solvents and gradients,that means without method optimization,totally different samples can be separated with outstanding separation power.Each sample was spiked with cyclophosphamide and ifosfamide and the ion suppression was determined by comparison of the peak area in the complex samples and in pure water after analysis of these samples with a 1D-LC and a 2D-LC approach.It is shown that the 2D-LC method allows an external calibration for the spiked compounds in the plant and waste water sample because of the higher separation power in comparison with 1D-LC.展开更多
文摘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。
文摘A two-dimensional LC(2D-LC)method was coupled to an ion mobility-high-resolution mass spectrometer(IM-MS),which enables the separation of complex samples in four dimensions[2D-LC,ion mobility(IM)and mass spectrometry(MS)].This approach works as a continuous multiheart-cutting LC-system,using a long modulation time of four minutes,in comparison to comprehensive two-dimensional liquid chromatography,which allows the complete transfer of most of the first dimension peaks to the second dimension column without fractionation.Hence,each compound delivers only one peak in the second dimension,which simplifies the data handling even when ion mobility as a third and mass spectrometry as a fourth dimension are introduced.The analysis of different complex samples,such as a plant extract from Hediotys diffusa and Scutellaria barbata,a waste water inflow,and a biocoal sample,was shown.The results of the four-dimensional separation method demonstrate that with the same column combination and the same solvents and gradients,that means without method optimization,totally different samples can be separated with outstanding separation power.Each sample was spiked with cyclophosphamide and ifosfamide and the ion suppression was determined by comparison of the peak area in the complex samples and in pure water after analysis of these samples with a 1D-LC and a 2D-LC approach.It is shown that the 2D-LC method allows an external calibration for the spiked compounds in the plant and waste water sample because of the higher separation power in comparison with 1D-LC.
