Synthesis and evaluation of porous polymethylsilsesquioxane microspheres as low silanol activity chromatographic stationary phase for basic compound separation

Huo, Zhixia; Wan, Qian-Hong; Chen, Lei

doi:10.1016/j.chroma.2018.04.024

Cited by 17 publications

(3 citation statements)

References 39 publications

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“…When the pH increased from pH 4.0 to 9.0, the I pa of matrine and sophoridine increased correspondingly ( Figure S4A,B ). Thus, the main mechanism was attributed to the property of matrine and sophoridine, which are alkaloid drugs with pK a value of about 7.80−8.20 [ 31 , 32 ]. Their structure contains a tertiary amine nitrogen atom ( 1 N), and an amide structure ( 2 N) which has alkalinity.…”

Section: Resultsmentioning

confidence: 99%

Construction of Multiple Switchable Sensors and Logic Gates Based on Carboxylated Multi-Walled Carbon Nanotubes/Poly(N,N-Diethylacrylamide)

Bai

et al. 2018

Sensors

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In this work, binary hydrogel films based on carboxylated multi-walled carbon nanotubes/poly(N,N-diethylacrylamide) (c-MWCNTs/PDEA) were successfully polymerized and assembled on a glassy carbon (GC) electrode surface. The electroactive drug probes matrine and sophoridine in solution showed reversible thermal-, salt-, methanol- and pH-responsive switchable cyclic voltammetric (CV) behaviors at the film electrodes. The control experiments showed that the pH-responsive property of the system could be ascribed to the drug components of the solutions, whereas the thermal-, salt- and methanol-sensitive behaviors were attributed to the PDEA constituent of the films. The CV signals particularly, of matrine and sophoridine were significantly amplified by the electrocatalysis of c-MWCNTs in the films at 1.02 V and 0.91 V, respectively. Moreover, the addition of esterase, urease, ethyl butyrate, and urea to the solution also changed the pH of the system, and produced similar CV peaks as with dilution by HCl or NaOH. Based on these experiments, a 6-input/5-output logic gate system and 2-to-1 encoder were successfully constructed. The present system may lead to the development of novel types of molecular computing systems.

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Section: Resultsmentioning

confidence: 99%

Construction of Multiple Switchable Sensors and Logic Gates Based on Carboxylated Multi-Walled Carbon Nanotubes/Poly(N,N-Diethylacrylamide)

Bai

et al. 2018

Sensors

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“…A mixed-mode reversedphase/weak cation exchange (carboxyl-form ion-exchange) was demonstrated in catecholamines and amphetamine related drugs [17]. Basic and acidic additives were utilized for the enantiomeric separation of some basic chiral drugs in polysaccharide-based chiral columns [19]. Furthermore, polymethylsilsesquioxane microspheres were synthesized for basic compounds as low silanol activity chromatographic stationary phase [19].…”

Section: Introductionmentioning

confidence: 99%

“…Basic and acidic additives were utilized for the enantiomeric separation of some basic chiral drugs in polysaccharide-based chiral columns [19]. Furthermore, polymethylsilsesquioxane microspheres were synthesized for basic compounds as low silanol activity chromatographic stationary phase [19].…”

Section: Introductionmentioning

confidence: 99%

Quantitative Explanation of Basic Compound Retention Mechanisms in Reversed-Phase Mode Liquid Chromatography

Hanai¹

2020

Preprint

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The quantitative analysis of the chromatographic behavior of basic compounds was performed in silico. The liquid chromatography (LC) data measured with pentyl-, hexenyl-, and octyl-bonded silica gels were analyzed in silico employing model phases. The main retention force was the van der Waals (VW) interaction, and the main desorption force was an electrostatic (ES) interaction. The contribution of hydrogen bonding (HB) was weak compared to that for acidic compounds. The quantitative explanation was achieved utilizing the calculated VW, HB, and ES energy values obtained from a molecular mechanics program. The electron localization was observed at the molecular interaction-site calculated MOPAC program. This fundamental approach was like that of explaining chemical reactions. The difference was electron localization in chromatography or electron transfer in a chemical reaction.

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Base‐deactivated and alkaline‐resistant chromatographic stationary phase based on functionalized polymethylsilsesquioxane microspheres

Huo

Chen

2019

J of Separation Science

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Vinyl, chloropropyl, and mercaptopropyl functionalized particles were prepared by a two‐step acidic/alkaline catalyzed co‐hydrolysis/condensation of methyltrimethoxysilane with a different silane precursor that carries chemically reactive functional group including vinyl, chloropropyl, and mercaptopropyl, respectively. The morphology, pore structure, and functional groups of the synthesized packings were studied by SEM, nitrogen adsorption‐desorption measurements, and solid‐state 13C 29Si NMR spectroscopy, respectively. The particles show ordered sphere, narrow particle size distribution, and mesoporous structure. The carbon contents of the microspheres are in the range of 17–19%, comparable to those of octadecyl‐bonded silica packings. The three‐kind of microspheres were directly used as packing materials for high‐performance liquid chromatography without size classification. The chromatographic performance of the columns was evaluated and compared with a commercially available C18 phase. The results revealed that these columns possess typical reversed‐phase chromatographic properties with increased hydrophobicity than polymethylsilsesquioxane and symmetric peaks for basic compounds. They were applied to the simultaneous separation of combination bendazol hydrochlorothiazide capsules containing polar and basic drugs with peaks identified by tandem with mass spectrometry. In general, a novel method is provided for the synthesis of different methyltrimethoxysilane‐derived microspheres for high‐performance liquid chromatography, which are advantageous for separating basic compounds.

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Synthesis and evaluation of porous polymethylsilsesquioxane microspheres as low silanol activity chromatographic stationary phase for basic compound separation

Cited by 17 publications

References 39 publications

Construction of Multiple Switchable Sensors and Logic Gates Based on Carboxylated Multi-Walled Carbon Nanotubes/Poly(N,N-Diethylacrylamide)

Construction of Multiple Switchable Sensors and Logic Gates Based on Carboxylated Multi-Walled Carbon Nanotubes/Poly(N,N-Diethylacrylamide)

Quantitative Explanation of Basic Compound Retention Mechanisms in Reversed-Phase Mode Liquid Chromatography

Base‐deactivated and alkaline‐resistant chromatographic stationary phase based on functionalized polymethylsilsesquioxane microspheres

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