2D-LC-Q-TOF-MS鉴定门冬氨酸钾镁注射液中的未知杂质  

Identification of the Unknown Impurity in Potassium Aspartate and Magnesium Aspartate Injection by 2D-LC-Q-TOF-MS

作　　者：林丽琴[1] 彭彦 金朦娜 高丽琼 汪霞 王秀秀 LIN Liqin;PENG Yan;JIN Mengna;GAO Liqiong;WANG Xia;WANG Xiuxiu(Hangzhou Institute for Food and Drug Control,Hangzhou 310022,China)

机构地区：[1]杭州市食品药品检验研究院,杭州310022

出　　处：《中国现代应用药学》2023年第19期2721-2727,共7页Chinese Journal of Modern Applied Pharmacy

摘　　要：目的通过中心切割二维液相色谱-飞行时间质谱联用技术(2D-LC-Q-TOF-MS)分离,鉴定门冬氨酸钾镁注射液中的未知杂质。方法采用Waters ACQUITY UPLC 2D超高效二维液相系统和Xevo G2-XS QTof-四极杆飞行时间质谱系统,一维液相色谱采用Agilent ZORBAX-NH2色谱柱,以0.05 mol·L^(-1)磷酸二氢钾溶液-乙腈(37∶63)为流动相,流速为1.3 mL·min^(-1),检测波长为200 nm;二维液相色谱采用Waters ACQUITY UPLC HSS T3色谱柱,以0.1%甲酸(ESI^(+))/5 mmol·L^(-1)甲酸铵(ESI^(-))为流动相A,以乙腈为流动相B,梯度洗脱;质谱采用电喷雾电离源(ESI),正负离子模式检测。结果通过高分辨质量数和二级质谱碎片,结合UNIFI软件,推测得到了门冬氨酸钾镁注射液中的未知杂质的可能结构。结论2D-LC-Q-TOF-MS可用于门冬氨酸钾镁注射液中杂质的在线定性鉴别,为门冬氨酸钾镁注射液的质量控制和工艺优化提供参考依据。OBJECTIVE To study the unknown impurity in potassium aspartate and magnesium aspartate injection by heart-cutting two-dimensional liquid chromatography coupled with Quadrupole time-of-flight mass spectrometry(2D-LC-Q-TOF-MS).METHODS The Waters ACQUITY UPLC 2D system and Xevo G2-XS QTof-MS system were used.One-dimensional chromatographic conditions were as listed.An Agilent ZORBAX-NH2 column was used,and potassium dihydrogen thophosphate(0.05 mol·L^(−1))-acetonitrile(37∶63)as the mobile phase,at a flow rate of 1.3 mL·min^(-1).The detection wavelength was set at 200 nm.Two-dimensional chromatographic conditions were as listed.A Waters ACQUITY UPLC HSS T3 column was used,and 0.1%formic acid solution(ESI^(+))/5 mmol·L^(−1) ammonium formate(ESI^(−))as the mobile phase A,and acetonitrile as the mobile phase B,in gradient mode.The mass spectrometry used an electro spray ionization source(ESI)for positive and negative ion mode detection.RESULTS Combined the high resolution mass,MS2 fragment ions and the UNIFI software,the possible structure of the unknown impurity in potassium aspartate and magnesium aspartate injection was infered.CONCLUSION The 2D-LC-Q-TOF-MS method can be used to identify impurities in potassium aspartate and magnesium aspartate injection,which provides reference for the improvement of quality control and process optimization of potassium aspartate and magnesium aspartate injection.

关 键 词：门冬氨酸钾镁注射液 杂质 中心切割 液相色谱-质谱联用 

分 类 号：R927.11[医药卫生—药学]