在线二维高效液相色谱-四极杆飞行时间质谱法分析两性霉素B的杂质谱
O658; 建立了基于在线二维高效液相色谱-四极杆飞行时间质谱(2D HPLC-Q TOF/MS)的两性霉素B杂质谱分析方法.第一维液相色谱(1D-LC)以XBridge Shield C18为色谱柱、甲醇-乙腈-4.2 g/L柠檬酸水溶液为流动相.第二维液相色谱(2D-LC)以Xtimate C8为捕集柱,以含0.1％甲酸的10 mmol/L甲酸铵水溶液-乙腈(95∶5,v/v)为流动相进行捕集和脱盐;以Xtimate C8为色谱柱,以含0.1％甲酸的10 mmol/L甲酸铵水溶液-乙腈为流动相进行洗脱.该方法结合了在线稀释和多针捕集装置,实现了 10个组分/杂质的高效分离,并通过四极杆飞行...
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| Published in | Sepu Vol. 42; no. 5; pp. 432 - 444 |
|---|---|
| Main Authors | , , , |
| Format | Journal Article |
| Language | Chinese English |
| Published |
No. 457, Zhongshan Road, Shahekou District, Dalian City, Liaoning Province
上海市食品药品检验研究院,上海 201203%上海市食品药品检验研究院,上海 201203%中国医药工业研究总院,上海 201203
08.04.2024
复旦大学药学院,上海 201203 Editorial board of Chinese Journal of Chromatography |
| Subjects | |
| Online Access | Get full text |
| ISSN | 1000-8713 1872-2059 |
| DOI | 10.3724/SP.J.1123.2023.07012 |
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| Abstract | O658; 建立了基于在线二维高效液相色谱-四极杆飞行时间质谱(2D HPLC-Q TOF/MS)的两性霉素B杂质谱分析方法.第一维液相色谱(1D-LC)以XBridge Shield C18为色谱柱、甲醇-乙腈-4.2 g/L柠檬酸水溶液为流动相.第二维液相色谱(2D-LC)以Xtimate C8为捕集柱,以含0.1％甲酸的10 mmol/L甲酸铵水溶液-乙腈(95∶5,v/v)为流动相进行捕集和脱盐;以Xtimate C8为色谱柱,以含0.1％甲酸的10 mmol/L甲酸铵水溶液-乙腈为流动相进行洗脱.该方法结合了在线稀释和多针捕集装置,实现了 10个组分/杂质的高效分离,并通过四极杆飞行时间质谱实现了对不稳定组分/杂质的结构推断,解决了 2D HPLC溶剂兼容性的难题,增加了分析通量,提高了 2D HPLC的自动化能力,避免了两性霉素B与部分杂质在色谱分离过程中相互转化的问题,提高了检测灵敏度.利用该方法可以灵敏地对两性霉素B的杂质谱进行分析,所得到的研究结果对两性霉素B的生产工艺改进具有指导意义. |
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| AbstractList | 建立了基于在线二维高效液相色谱-四极杆飞行时间质谱(2D HPLC-Q TOF/MS)的两性霉素B杂质谱分析方法。第一维液相色谱(1D-LC)以XBridge Shield C18为色谱柱、甲醇-乙腈-4.2 g/L柠檬酸水溶液为流动相。第二维液相色谱(2D-LC)以Xtimate C8为捕集柱,以含0.1%甲酸的10 mmol/L甲酸铵水溶液-乙腈(95∶5, v/v)为流动相进行捕集和脱盐;以Xtimate C8为色谱柱,以含0.1%甲酸的10 mmol/L甲酸铵水溶液-乙腈为流动相进行洗脱。该方法结合了在线稀释和多针捕集装置,实现了10个组分/杂质的高效分离,并通过四极杆飞行时间质谱实现了对不稳定组分/杂质的结构推断,解决了2D HPLC溶剂兼容性的难题,增加了分析通量,提高了2D HPLC的自动化能力,避免了两性霉素B与部分杂质在色谱分离过程中相互转化的问题,提高了检测灵敏度。利用该方法可以灵敏地对两性霉素B的杂质谱进行分析,所得到的研究结果对两性霉素B的生产工艺改进具有指导意义。 O658; 建立了基于在线二维高效液相色谱-四极杆飞行时间质谱(2D HPLC-Q TOF/MS)的两性霉素B杂质谱分析方法.第一维液相色谱(1D-LC)以XBridge Shield C18为色谱柱、甲醇-乙腈-4.2 g/L柠檬酸水溶液为流动相.第二维液相色谱(2D-LC)以Xtimate C8为捕集柱,以含0.1％甲酸的10 mmol/L甲酸铵水溶液-乙腈(95∶5,v/v)为流动相进行捕集和脱盐;以Xtimate C8为色谱柱,以含0.1％甲酸的10 mmol/L甲酸铵水溶液-乙腈为流动相进行洗脱.该方法结合了在线稀释和多针捕集装置,实现了 10个组分/杂质的高效分离,并通过四极杆飞行时间质谱实现了对不稳定组分/杂质的结构推断,解决了 2D HPLC溶剂兼容性的难题,增加了分析通量,提高了 2D HPLC的自动化能力,避免了两性霉素B与部分杂质在色谱分离过程中相互转化的问题,提高了检测灵敏度.利用该方法可以灵敏地对两性霉素B的杂质谱进行分析,所得到的研究结果对两性霉素B的生产工艺改进具有指导意义. |
| Abstract_FL | Amphotericin B(AmB)is a polyene-macrolide antimicrobial drug with a broad anti-bacterial spectrum and remarkable efficacy against deep fungal infections.It binds to ergosterol on the fungal cell membrane and alters its permeability,thereby destroying the membrane.AmB is a multicomponent antimicrobial medication that contains a wide range of impurities,render-ing quality analysis extremely difficult.In the current Chinese Pharmacopoeia(Edition 2020)and European Pharmacopoeia(EP10.3),high performance liquid chromatography(HPLC)is applied to examine related substances in AmB.However,this technique presents a number of issues.For instance,the mobile phases used in the HPLC method described in both references contain nonvolatile inorganic salts,which cannot be coupled with a mass spectrometry(MS)detector.In addition,because the mobile phases used have a low pH,the component/impuri-ties of AmB drug can easily be degraded or interconverted during the analytical process,leading to reduced analytical accuracy.Therefore,the accuracy and sensitivity of this method must be improved.In this study,a method based on on-line two-dimensional high performance liquid chromatography-quadrupole time-of-flight mass spectrometry(2D HPLC-Q TOF/MS)was de-veloped to analyze the impurity profile of AmB in accordance with the Chinese Pharmacopoeia(Edition 2020)and European Pharmacopoeia(EP10.3).The method combines on-line dilution and a multiple-capture HPLC system to achieve the efficient separation of AmB component/im-purities.It also resolves the issue of poor solvent compatibility in 2D HPLC,increases the ana-lytical flux,enhances the automation capability,reduces the mutual conversion of AmB and its impurities during the analytical process,and increases the detection sensitivity of the method.MS was also used to determine the structural inference of unstable components and impurities.An XBridge Shield C18 column(250 mm×4.6 mm,3 μm)was used for first-dimensional-liquid chromatography with gradient elution using methanol-acetonitrile-4.2 g/L citric acid mono-hydrate solution(10∶30∶60,v/v/v,pH 4.7)as mobile phase A and methanol-acetonitrile-4.2 g/L citric acid monohydrate solution(12∶68∶20,v/v/v,pH 3.9)as mobile phase B.An Xtimate C8 column(10 mm×2.1 mm,5 μm)was used as the trap column,and trapping and desalting were performed using 10 mmol/L ammonium formate aqueous solution containing 0.1％formic acid-acetonitrile(95∶5,v/v).An Xtimate C8 column(250 mm×2.1 mm,5 μm)was used for second-dimensional-liquid chromatography with gradient elution using 10 mmol/L ammonium formate aqueous solution containing 0.1％formic acid-acetonitrile(95∶5,v/v)and 10 mmol/L ammonium formate aqueous solution containing 0.1％formic acid-acetonitrile(5∶95,v/v)as mobile phases.The data were collected in positive-ion mode.In this study,the structures of six impurities in amphotericin B were inferred,according to the fragmentation,the MS and MS2 spectra of each impurity.The developed method can be used to quickly and sensitively analyze the impurity profile of AmB.Furthermore,the research results on impurity profiles can be applied to guide improvements in AmB production. |
| Author | 翁荣文 刘浩 闻宏亮 王轩堂 |
| AuthorAffiliation | 复旦大学药学院,上海 201203;上海市食品药品检验研究院,上海 201203%上海市食品药品检验研究院,上海 201203%中国医药工业研究总院,上海 201203 |
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| Author_FL | WENG Rongwen WANG Xuantang LIU Hao WEN Hongliang |
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| DocumentTitle_FL | Impurity profile analysis of amphotericin B using on-line two-dimensional high performance liquid chromatography-quadrupole time-of-flight mass spectrometry |
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| Keywords | 两性霉素B on-line two-dimensional high performance liquid chromatography-quadrupole time-of-flight mass spectrometry(2D HPLC-Q TOF/MS) impurity profile amphotericin B 在线二维高效液相色谱-四极杆飞行时间质谱 杂质谱 |
| Language | Chinese English |
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| Publisher | 上海市食品药品检验研究院,上海 201203%上海市食品药品检验研究院,上海 201203%中国医药工业研究总院,上海 201203 复旦大学药学院,上海 201203 Editorial board of Chinese Journal of Chromatography |
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| Title | 在线二维高效液相色谱-四极杆飞行时间质谱法分析两性霉素B的杂质谱 |
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