Nano-liquid chromatography with monolithic stationary phase based on naphthyl monomer for proteomics analysis

Aydoğan, Cemil; Beltekin, Büşra; Alharthi, Sarah; Ağca, Can Ali; Erdoğan, İbrahim Y.

doi:10.1016/j.chroma.2023.463804

Cited by 9 publications

(4 citation statements)

References 26 publications

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“…The monolithic silica sorbent had well-defined macro/mesoporous structures with characteristic cocontinuous silica frameworks in a micrometer scale (Figure a). , It is an high-performance LC (HPLC) sorbent with high mechanical rigidity like a sintered glass filter. − LC purification using the monolithic silica column with a halogen-free HEX/toluene solution as the developing solvent was allowed without any deposits and clogging in the column sorbent (Figure b), due to meta-stabilized supersaturation as described below. The retention behavior of the mixture of DACT-II in the monolithic silica was the same for conventional thin-layer chromatography (TLC) plates, enabling a simple fraction collection (Figure S1 and Table S1).…”

Section: Resultsmentioning

confidence: 99%

Halogen-Free Purification of Low-Solubility Compounds in Supersaturated Liquid Chromatography Using Monolithic Silica

Miyamoto,

Kanamori,

Nakagawa

et al. 2024

ACS Sustainable Chem. Eng.

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Chemical syntheses on the cutting edge of advanced science involve several purification techniques to satisfy product purity and reduce costs and environmental impacts. Liquid chromatography (LC) purification has been one of the most important purification techniques for many organic compounds, which involves technical problems such as increasing LC wastes and the inevitable use of harmful halogenated solvents for the separation of low-solubility compounds. Herein, we report a halogen-free purification method in LC to eliminate contamination risks and environmental emissions of harmful halogenated solvents with satisfactory LC productivity by introducing monolithic silica columns. The purification of an organic light-emitting diode material of 9-[4-(4,6-diphenyl-1,3,5-triazin-2-yl)phenyl]-N,N,N′,N′-tetraphenyl-9H-carbazole-3,6-diamine with an n-hexane/toluene solution as the developing solvent is allowed without any deposits and clogging in the monolithic silica column even in low-solubility conditions. The meta-stabilized supersaturation in the column due to the cocontinuous macroporous structure of the monolith allows halogen-free LC purification and consecutive, spontaneous recrystallization of the target product. Achieving high yield and purity, 61% and 99.92%, respectively, leads to "zero emissions" of harmful LC wastes when combined with reduced solvent usage, column reusability, and solvent recycling. This zerowaste strategy by the high-performance LC column for bulk purification minimizes the cost and energy involved in many purification processes, achieving both high-purity purification and reduction of environmental risks.

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Section: Resultsmentioning

confidence: 99%

Halogen-Free Purification of Low-Solubility Compounds in Supersaturated Liquid Chromatography Using Monolithic Silica

Miyamoto,

Kanamori,

Nakagawa

et al. 2024

ACS Sustainable Chem. Eng.

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“…In contrast to the classical silica particles, monolithic porous silica can be regarded as an alternative sorbent with a rigid skeletal structure similar to that of a sintered glass filter. The monolithic silicas have controllable macro/mesoporous structures with characteristic cocontinuous silica frameworks on the micrometer scale and have been investigated since the 1990s. − The size-controlled pore structures of the monolith enable it to provide an excellent separation performance in LC. − Rapid mass transfer of monolithic columns with low back-pressure compared with the particle-packed column has been revealed due to the cocontinuous macroporous structure with high porosity. − The monolith columns are commercialized as Chromolith, showing high column durability with a long lifetime of >1000 repetitions. − Fabrications of a large-volume monolithic column exceeding 1000 mL have been achieved, and the monoliths showed the possibility of improved column efficiency for purification processes …”

Section: Introductionmentioning

confidence: 99%

Significant Waste Reduction in Liquid Chromatography by a Reusable Large-Volume Monolithic Silica Column

Miyamoto,

Kanamori,

Nakagawa

et al. 2024

ACS Sustainable Chem. Eng.

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The highly efficient separation of product mixtures in chemical synthesis is increasingly crucial for realizing sustainable chemical processes. Here, we report that large-volume monolithic silica with a well-defined cocontinuous porous structure brings significant benefits to liquid chromatography, satisfying both the enhanced efficiency and remarkable reduction of chromatographic wastes of solvent and solid separation media. Reusability of the monolithic silica column has been demonstrated by regeneration with an acid-flow washing, in which the cocontinuous porous structure of monolithic silica is well retained even in aqua regia in the regeneration process. The resolution of separation is comparable to preparative high-performance liquid chromatography, and the extremely low column back-pressure is suitable for open and flash columns. Moreover, a good correlation of the retention with conventional thin-layer chromatography and the high loading capacity up to 10 wt % are advantageous in overloading purification. Improved productivity with the large-volume monolithic silica has been confirmed in the practical purification of a low-solubility compound, 9-[4-(4,6-diphenyl-1,3,5-triazin-2-yl)phenyl]-N,N,N′,N′-tetraphenyl-9H-carbazole-3,6-diamine (DACT-II), for a highly efficient organic light-emitting diode. Reduction of solvent and solid consumption by 60 and 90%, respectively, with increased purities in each step of the total synthesis of DACT-II, has been demonstrated in comparison with purification with standard silica particles.

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“…The rapid development in promising technologies, such as advanced chromatography and nuclear magnetic resonance (NMR), is reflected in new developments in instrumentation that improve resolution, sensitivity, and speed. These advances enable improved molecule detection and quantitation under in vivo as well as in vitro conditions [ 4 , 5 , 6 , 7 ]…”

Section: Introductionmentioning

confidence: 99%

Nano-Liquid Chromatography with a New Monolithic Column for the Analysis of Coenzyme Q10 in Pistachio Samples

et al. 2023

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Coenzyme Q10 (CoQ10) is a vital substance found throughout body. It helps convert food into energy and is eaten small amounts in foods. CoQ10 has gained great interest in recent years as a potential candidate for the treatment of various diseases. The content of CoQ10 in food samples is a crucial quality index for foods. Therefore, the development of sensitive separation and quantification method for determining the amount of CoQ10 in various samples, especially in foods, is an important issue, especially for food nutrition. In this study, a new, miniaturized monolithic column was developed and applied for the determination of CoQ10 in pistachio samples by nano-liquid chromatography (nano-LC). The monolithic column with a 50 µm i.d. was prepared by in situ polymerization using laurylmethacrylate (LMA) as the main monomer and ethylene dimethacrylate (EDMA) as the crosslinker. Methanol (MeOH) and polyethyleneglycol (PEG) were used as porogenic solvents. The final monolithic column was characterized by using scanning electron microscopy (SEM) and chromatographic analyses. The monolithic column with a 50 µm i.d. was applied to the analysis of CoQ10 in pistachio samples in nano-LC. This analytical method was validated by means of sensitivity, linearity, precision, recovery, and repeatability. The LOD and LOQ values were 0.05 and 0.48 µg/kg, respectively. The developed method using the monolithic column was optimized to achieve very sensitive analyses of CoQ10 content in the food samples. The applicability of the method was successfully demonstrated by the analysis of CoQ10 in pistachio samples.

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Nano-liquid chromatography with monolithic stationary phase based on naphthyl monomer for proteomics analysis

Cited by 9 publications

References 26 publications

Halogen-Free Purification of Low-Solubility Compounds in Supersaturated Liquid Chromatography Using Monolithic Silica

Halogen-Free Purification of Low-Solubility Compounds in Supersaturated Liquid Chromatography Using Monolithic Silica

Significant Waste Reduction in Liquid Chromatography by a Reusable Large-Volume Monolithic Silica Column

Nano-Liquid Chromatography with a New Monolithic Column for the Analysis of Coenzyme Q10 in Pistachio Samples

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