Safety Monitoring

Fragment ions analysis of 24 phthalates based on electrospray electrostatic orbitrap mass spectrometry

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  • Research Institute of Jiangsu Hansoh Pharmaceutical Group Co., Ltd., Lianyungang 222069, China

Received date: 2022-09-29

  Online published: 2024-06-24

Abstract

Objective: Based on the structural identification requirements of unknown extracts and leachables in compatibility studies, the mass spectrometry information of 24 phthalate compounds was collected. The structure, morphology and fragmentation pathway of each fragment ion were analyzed in view of the advantage of high resolution orbitrap mass spectrometry. Methods: The qualitative determination was carried out by ultra-high performance liquid chromatography-quadrupole/electrostatic orbitrap mass spectrometry. The column was Agilent Proshell 120EC-C18 column (100 mm×4.6 mm, 2.7 μm), and the mobile phase A was 0.1% acetic acid aqueous solution, B was methanol, C was acetonitrile. Gradient elution with flow rate 1.0 mL·min-1 was used. Ionization mode was ESI+ and spray voltage was 3 500 V. Meanwhile, sheath gas flow rate was 7 L·min-1 and auxiliary gas flow rate was 12 L·min-1. The temperature of ion transfer tube and ion source were 325 ℃ and 320 ℃, respectively. The resolution was 120000. Results: The 24 phthalate compounds had good primary mass spectrometry responses, and [M+H]+ ions were clearly visible. Secondary fragment ions were evenly distributed at high, medium and low mass-to-charge ratios. Strong characteristic peak of m/z 149 was accompanied by other ions such as m/z 167, 121, 111, and 93. Benefiting from the systematic summary of fragment ions of single reference solution, the structure analysis of phthalates detected in the sample solution was completed. Conclusion: In this study, the advantage of high-resolution electrospray electrostatic orbitrap mass spectrometry was used to comprehensively elucidate the characteristic ions of typical phthalates, as well as their forms and sources. The detected unknown extracts and leachables in the materials of common compatibility studies showed the importance of in-depth understanding of the mass spectrometry characteristics of phthalates. It could provide a reliable reference for the characterization of unknown extracts and leachables in compatibility studies from both theoretical analysis and practical applications, especially the structural identification of unknown impurities of phthalates.

Cite this article

MA Neng-xuan, WU Meng-xue, YANG Bao-hai, GU Chen-chen, ZHAO Nan-nan . Fragment ions analysis of 24 phthalates based on electrospray electrostatic orbitrap mass spectrometry[J]. Chinese Journal of Pharmaceutical Analysis, 2023 , 43(9) : 1543 -1552 . DOI: 10.16155/j.0254-1793.2023.09.12

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