Citation: QIU Ya, QIN Feng, WEN Hongliang, ZHAO Jingdan, LIU Hao, YANG Meicheng. Impurity profile study of cefalotin sodium by two-dimensional liquid chromatography-quadrupole time-of-flight mass spectrometry[J]. Chinese Journal of Chromatography, ;2015, 33(12): 1314-1319. doi: 10.3724/SP.J.1123.2015.07027 shu

Impurity profile study of cefalotin sodium by two-dimensional liquid chromatography-quadrupole time-of-flight mass spectrometry

1.
Shanghai Institute for Food and Drug Control, Shanghai 201203, China

Corresponding author: YANG Meicheng,
Received Date: 27 July 2015

Fund Project: 中国食品药品检定研究院中青年发展研究基金项目(2013WA4). (2013WA4)

A two-dimensional liquid chromatography-quadrupole time-of-flight mass spectrometry (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 chromatography, with gradient elution using pH 2.5 phosphate buffer and acetonitrile as the mobile phases. 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 second dimensional chromatography, with gradient elution using water containing 0.1% (v/v) formic 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 1000 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 impurities 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.
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通讯作者: 陈斌, bchen63@163.com

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沈阳化工大学材料科学与工程学院沈阳 110142

Impurity profile study of cefalotin sodium by two-dimensional liquid chromatography-quadrupole time-of-flight mass spectrometry

南开大学师唯/华北电力大学（保定）刘景维：二维配位聚合物中有序的亲锂冠醚位点用于无枝晶锂沉积

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通讯作者: 陈斌, bchen63@163.com