摘要 采用柱切换二维色谱方法的原理，在一维上对药物的有关物质进行完全基线分离后，对大于0.1%的含量的杂质，切入到二维系统中，进行在线除盐后，进MS进行鉴定。本方法以阿莫西林中的有关杂质进行分析为例，采用Ultimate DGP3600二维色谱与三重四极杆质谱仪TSQ Vantage 联用，正/负离子同时扫描测定，同时对确定的母离子再进行子离子扫描，以推测相关的结构信息。右泵为一维分析泵，分析柱Acclaim C18柱（150 mm×4.6 mm, 5 μm），含非挥发性盐流动相，流速1.0mL/min；左泵，接二维在线除盐分析柱Acclaim PA2柱（3.0 mm×50mm, 3 μm），含挥发性盐溶液流动相兼容MS，流速0.3mL/min；柱温：30℃；进样量：20 μL ；检测波长：230 nm。结果表明，在不改变阿莫西林国家药典标准方法的前提下，通过柱切换在线除盐技术使得分析条件能够兼容质谱并鉴定出阿莫西林中4种杂质，因此，本研究可以指导阿莫西林化工生产过程中杂质的限量，值得推广应用。
Abstract: Based on the principle of two-dimensional chromatograph, related impurities more than 0.1% of drug were desalted and then switched to the second dimension for identification using MS after complete baseline separation in the first dimension. Taking amoxicillin as an example, we used Ultimate DGP3600 two-dimensional chromatography coupled with three-triple quadrupole mass spectrometer (TSQ Vantage), while the positive / negative ions were being scanned at the same time. Furthermore, the parent ions were scanned followed by determination of the daughter ions so as to speculate the related structure information. The right pump was one-dimensional analysis of pump and the analytical column was Acclaim C18 column (150 mm × 4.6 mm, 5 μm), containing non-volatile salt mobile phase, with flow rate of 1.0 mL/min; the left pump was connected to D-dimensional online desalting analytical column Acclaim PA2 column (3 mm × 50mm, 3 μm), the mobile phase containing volatile salt solution being compatible with MS, flow rate was 0.3 mL/min; column temperature was 30 ℃; sample was injected 20 μL; the detected wavelength was 230 nm. It was shown that, abiding by national pharmacopoeia standard method, four kinds of impurities in amoxicillin were identified by column-switching online desalting method combined with mass spectrometry. Therefore, our study would be benefit for limited control of amoxicillin during the process of chemical production, being worthy of popularization.
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