Journals / Hacettepe Journal of Biology and Chemistry / 2018 / Cilt: 46 - Sayı: 1

Synthesis and Characterisation of a New Hydrophilic Interaction/Reversed Phase Mixed-Mode Chromatographic Stationary Phase

Yeni bir Hidrofilik Etkileşim/Ters Faz Karışık-Mod Sıvı Kromatografik Sabit Fazın Sentezi ve Karakterizasyonu

Pages
43–52
Publication Date
2022-10-17
DOI
—
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AI Summary & Key Takeaways

AI Insight
⚡ TL;DR(Too Long; Didn't Read)

The stationary phase has also chirality and can be used in enantioseparation of racemic compounds in normal phase chromatography (NPLC).

📌 3 Key Takeaways

🎯
Objective & Hypothesis:Anovel multifunctional stationary phase based the amide-silica was synthesised starting from L-isoleucine and 2-aminoacetanilide.
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Key Findings & Data:Hereby, compounds 1, 2, 3 and 4 were synthesised for the first time and 1, 2 and 4 were identified.
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Conclusion & Impact:The stationary phase has also chirality and can be used in enantioseparation of racemic compounds in normal phase chromatography (NPLC).
🔬Design:Research Article
📍Scope:Comprehensive Sample
⚙️Variables:Domain Parameters

Abstract

Anovel multifunctional stationary phase based the amide-silica was synthesised starting from L-isoleucine and 2-aminoacetanilide. Hereby, compounds 1, 2, 3 and 4 were synthesised for the first time and 1, 2 and 4 were identified. The stationary phase was synthesised by a reliable and repeatable method and characterized by elemental analysis, solid state 13C NMR, scanning electron microscope (SEM), and Brunauer, Emmett and Teller (BET). This stationary phase possess four amide groups as polar cites, phenyl ring as aromatic non-polar cite and isopropyl as an aliphatic non-polar cite. Therefore, it can act as both hydrophilic interaction (HILIC) and reversed phase (RPLC) chromatographic stationary phase. The stationary phase has also chirality and can be used in enantioseparation of racemic compounds in normal phase chromatography (NPLC).

Özet

L-izolözin ve 2-aminoasetanilitten yola çıkılarak amid-silika tabanlı çok fonksiyonlu yeni bir dolgu maddesi sentezlendi. Bu vesile ile bileşik 1, 2, 3 ve 4 ilk kez sentezlenmiş olup bileşik 1, 2 ve 4’ün ayrıntılı karakterizasyonları yapılmıştır. Dolgu maddesi güvenilir ve tekrarlanabilir bir yöntemle sentezlenmiş olup yapısı katı faz 13C NMR, taramalı elektron mikroskobisi (SEM), ve Brunauer, Emmett and Teller (BET) ile doğrulandı. Yeni geliştirilen bu dolgu maddesi polar grup olarak dört amid grubu, apolar gruplar olarak da aromatik halka ve alifatik zincir içerir. Bu nedenle, bu dolgu maddesi hem hidrofilik etkileşim (HILIC) hem de ters faz (RPLC) sıvı kromatografisinde kullanılabilir. Dolgu maddesinin L-izolözinden sentezlendiği için aynı zamanda kiraldir ve normal faz kromatografide rasemik bileşiklerin enantiyomerik ayrılmasında kullanılabilir.

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Cite This Article

ARAL, H. (2022). Synthesis and Characterisation of a New Hydrophilic Interaction/Reversed Phase Mixed-Mode Chromatographic Stationary Phase. Hacettepe Journal of Biology and Chemistry, Cilt: 46 - Sayı: 1, 43–52. https://ajindex.com/articles/529049

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References (12)

  1. A.S. Feste, I. Khan, Separation of glucooligosaccharides and polysaccharide hydrolysates by gradient elution hydrophilic interaction chromatography with pulsed amperometric detection, J. Chromatogr., 630 (1992) 129-139.
  2. Y. Zhao, H.C. Law, Z. Zhang, H.C. Lam, Q. Quan, G. Li, et al., Online coupling of hydrophilic interaction/ strong cation exchange/reversed-phase liquid chromatography with porous graphitic carbon liquid chromatography for simultaneous proteomics and N-glycomics analysis, J. Chromatogr. A, 1415 (2015) 57-66.
  3. X. Liu, C.A. Pohl, Comparison of reversed-phase/ cation-exchange/anion-exchange trimodal stationary phases and their use in active pharmaceutical ingredient and counterion determinations, J. Chromatogr. A, 1232 (2012) 190-195.
  4. X. Liu, C. Pohl, A. Woodruff, J. Chen, Chromatographic evaluation of reversedphase/anion-exchange/cationexchange trimodal stationary phases prepared by electrostatically driven self-assembly process, J. Chromatogr. A, 1218 (2011) 3407-3412.
  5. X. Liu, C.A. Pohl, HILIC behavior of a reversed-phase/ cation-exchange/anionexchange trimode column, J. Sep. Sci., 33 (2010) 779-786.
  6. H. Hinterwirth, M. Lammerhofer, B. Preinerstorfer, A. Gargano, R. Reischl, W. Bicker, et al., Selectivity issues in targeted metabolomics: separation of phosphorylated carbohydrate isomers by mixedmode hydrophilic interaction/ weak anion exchange chromatography, J. Sep. Sci., 33 (2010) 3273–3282.
  7. X. Liu, C. Pohl, New hydrophilic interaction/ reversed-phase mixed-mode stationary phase and its application for analysis of nonionic ethoxylated surfactants, J. Chromatogr. A, 1191 (2008) 83–89.
  8. T. Saga, Y. Inoue, K. Yamaguchi, Determination of carbohydrates by hydrophilic interaction chromatography with pulsed amperometric detection using postcolumn pH adjustment, J. Chromatogr. A, 625 (1992) 151-155.
  9. Q. W. Yu, B. Lin, Y. Q. Feng, F. P. Zou, Application of humic acid bonded‐silica as a hydrophilic‐interaction chromatographic stationary Phase in separation of polar compounds, J. Liq. Chromatogr. Related. Technol., 31 (2008) 64-78.
  10. M.A. Strege, Hydrophilic interaction chromatography− electrospray mass spectrometry analysis of polar compounds for natural product drug discovery, Anal. Chem., 70 (1998) 2439-2445
  11. B.Y. Zhu, C.T. Colin, R.S. Hodges, Hydrophilicinteraction chromatography of peptides on hydrophilic and strong cation-exchange columns, J. Chromatogr., 548 (1991) 13-24.
  12. M.A. Strege, S. Stevensen, S. M.Lawrence, Mixed-mode anion−cation exchange/hydro