色谱Issue(12)：1314-1319,6.DOI:10.3724/SP.J.1123.2015.07027
在线二维液相色谱-四极杆飞行时间质谱法检测头孢噻吩钠的杂质谱
Impurity profile study of cefalotin sodium by two-dimensional liquid chromatography-quadrupole time-of-flight mass spectrometry
摘要
Abstract
A two-dimensional liquid chromatography-quadrupole time-of-flight mass spectrome-try(2D-LC-QTOF MS)method to profile the impurities of cefalotin sodium was developed. A Symmetry C18 column(250 mm×4. 6 mm,5 μm)was used in the first dimensional chromatog-raphy,with gradient elution using pH 2. 5 phosphate buffer and acetonitrile as the mobile pha-ses. The column temperature was maintained at 40 ℃ with an ultraviolet detection of 220 nm for analysis. An ACQUITY UPLC BEH C18 column(50 mm×2. 1 mm,1. 7 μm)was used in the sec-ond dimensional chromatography,with gradient elution using water containing 0. 1%( v/v)for-mic acid and acetonitrile containing 0. 1%( v/v)formic acid as the mobile phases. The column temperature was maintained at 40 ℃. An HLB C18 column(30 mm×2. 1 mm,20 μm)was used as the trap column. The data were collected in positive ion mode. The ion source temperature was set at 100 ℃ and the electrospray ionization( ESI)needle voltage was set at 1 000 V. The nebulizer gas temperature was set at 500 ℃. The molecular formulas of the impurities were determined by their exact masses and isotope distributions. And the structures were determined by the protonated molecular ions and the manufacturing process of cefalotin sodium. Six impu-rities of cefalotin sodium were characterized and the origination of the impurities was deduced. Three of them were unknown impurities to the best of our knowledge. It was confirmed that the Chinese Pharmacopoeia 2010 has mistaken impurity A of cefalotin sodium. The results indicated that the 2D-LC-QTOF MS method could be used to investigate the impurity profile of cefalotin sodium,and it is simple and sensitive.关键词
二维液相色谱-四极杆飞行时间质谱/杂质谱/头孢噻吩钠Key words
two-dimensional liquid chromatography-quadrupole time-of-flight mass spectrome-try(2D-LC-QTOF MS)/impurity profile/cefalotin sodium分类
化学化工引用本文复制引用
裘亚,秦峰,闻宏亮,赵敬丹,刘浩,杨美成..在线二维液相色谱-四极杆飞行时间质谱法检测头孢噻吩钠的杂质谱[J].色谱,2015,(12):1314-1319,6.基金项目
中国食品药品检定研究院中青年发展研究基金项目（2013WA4）． （）
