Analysis of Related Substances in Estramustine Phosphate Capsules by Heart-cutting Two-dimensional Liquid Chromatography-tandem Mass Spectrometry

DENG Yunfei1,2, WANG Linbo2, WU Xiaoluan2*, PENG Xingsheng1,2, LIN Mei1,2

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主办：上海医药工业研究院
　　　中国药学会
　　　中国化学制药工业协会
ISSN 1001-8255   CN 31-1243/R   ZYGZEA
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Chinese Journal of Pharmaceuticals
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Chinese Journal of Pharmaceuticals ›› 2018, Vol. 49 ›› Issue (11) : 1571. DOI: 10.16522/j.cnki.cjph.2018.11.014
Paper

Analysis of Related Substances in Estramustine Phosphate Capsules by Heart-cutting Two-dimensional Liquid Chromatography-tandem Mass Spectrometry

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Abstract

A heart-cutting and two-dimensional liquid chromatography was used by transferring the target component in estramustine phosphate (EMP) capsules through a loop which could achieve the purpose of on-line purification. In the two-dimensional liquid chromatography system, a C18 column was employed in the first dimension to separate the EMP. The target compound fluent were heart-cutted to a loop which was connected to a 6-way valve. Then the valve switched, so the second dimensional mobile phase took the target compound for the second dimension. Electrospray ionization source was operated in positive and negative ion mode. The structures of the related substances in EMP capsules were speculated by quadrupole time-of-flight (TOF) tandem mass spectrometry for accurate ion mass determination and by Q-TOF for product ion scanning. The structures of five related substances in EMP capsules were speculated according to the products of mass spectra fragmentation elucidation, combined with the synthetic process and stress testing results. Our work might provide some references for the quality control of EMP capsules.

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estramustine phosphate / related substance / two-dimensional liquid chromatography / heart-cutting / quadrupole time-of-flight tandem mass spectrometry

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DENG Yunfei1,2, WANG Linbo2, WU Xiaoluan2*, PENG Xingsheng1,2, LIN Mei1,2. Analysis of Related Substances in Estramustine Phosphate Capsules by Heart-cutting Two-dimensional Liquid Chromatography-tandem Mass Spectrometry. Chinese Journal of Pharmaceuticals. 2018, 49(11): 1571 https://doi.org/10.16522/j.cnki.cjph.2018.11.014

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