Recycling gradient-elution liquid chromatography for the analysis of chemical-composition distributions of polymers

Niezen, Leon E.; Staal, Bastiaan; Lang, Christiane; Philipsen, H. J. A.; Pirok, Bob W.J.; Somsen, Govert W.; Schoenmakers, Peter J.

doi:10.1016/j.chroma.2022.463386

Cited by 8 publications

(6 citation statements)

References 52 publications

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“…As an alternative, a so-called twin-column approach was later developed for analytical HPLC in which separation is carried out by flipping analytes between two columns without a need for passage through the pump [26]. This approach has gained popularity with several alternative applications described in the literature [27][28][29][30]. Aside from a need for a second column, however, this approach doubles the back pressure, which may pose a problem for the columns as well as a detector placed inside the high-pressure recycling loop.…”

Section: Resultsmentioning

confidence: 99%

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Improvement of oligonucleotide separation using a repetto high‐performance liquid chromatography recycling approach

Fiserova,

Minarik,

Nahunek

et al. 2024

J of Separation Science

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A new approach for the improvement of separation of oligonucleotides by recycling ion‐pairing chromatography is described. In the so‐called repetto process, segments of separated compounds are sequentially returned to the inlet for multiple passages through the column without a need to pass a pump and with the possibility of detecting the level of separation between individual passages. Unlike in the recently described twin‐column recycle approach in which eluents are repeatedly transferred between two separation columns, with the repetto method a single column is sufficient, and the detector is not exposed to high back pressure. The repetto principle was used for the separation of synthetic oligonucleotides, resulting in a multi‐fold improvement in single nt resolution of long (> 50 nt) synthetic oligonucleotide fragments with high gas chromatography (guanine‐cytosine) content > 40% and their separation from impurities of the original synthesis.

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Section: Resultsmentioning

confidence: 99%

“…A schematic illustration of the repetto recycling approach based on using synchronized switching of two 4‐port valves with a column and detector inside a closed loop. The complete principle, including a detailed description of valve connections, is described [30]. …”

Section: Resultsmentioning

confidence: 99%

Improvement of oligonucleotide separation using a repetto high‐performance liquid chromatography recycling approach

Fiserova,

Minarik,

Nahunek

et al. 2024

J of Separation Science

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“…A solid‐phase extraction‐MS platform used for monitoring secretion of glucose regulating hormones from human islet of Langerhans samples utilized an Arduino to control the 10‐port valve used for dual‐loop sample introduction [61]. Actuation of a 10‐port valve using an Arduino was also reported for a recycling chromatography system designed for polymer analysis [62]. Automated control of a miniaturized CE system meant for operation in extraterrestrial settings was achieved using a Teensy microcontroller [63].…”

Section: Autosamplers Valving and Other System Controlmentioning

confidence: 99%

The utilization of open‐source microcontroller boards and single‐board computers in liquid chromatography

Piccolo,

Foster,

Parker

et al. 2024

J of Separation Science

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Electronic system control of analytical instrumentation remains a critical aspect of modern measurement science. Within the field of liquid chromatography (LC), this is especially relevant for automation, module operation, detection, data acquisition, and data analysis. Increasingly, home‐built analytical tools used for liquid‐phase separations rely upon open‐source microcontrollers and single‐board computers to aid in simplifying these operations. In this review, we detail literature reported within the past 5 years in which these types of devices were used to advance various aspects of the LC research field, including sample preparation, instrument control, and data collection.

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“…One approach to determine polymer end groups is using interactive polymer chromatography (IPC), in which retention in IPC is often dependent on the chemical composition, functionality, and molecular weight of the polymer. [12][13][14][15][16][17][18][19][20] More specifically, interaction gradient elution polymer chromatography (interactive GPEC). [17,[21][22][23] In interactive polymer LC, the retention is governed by the polymer interaction with the chemical groups of the chromatographic column's stationary phase, and the polarity and elution strength of the mobile phase.…”

Section: Introductionmentioning

confidence: 99%

“…Normal phase and reversed phase gradient chromatography methods are often applied. [12][13][14][15][16][17][18][19][20] Previous research reported the use of interactive GPEC for the characterization of low molecular weight (<4000 Da) aromatic polyester from condensation reactions. Phillipsen et al used shallow gradients in interaction GPEC separations using normal-phase chromatography.…”

Section: Introductionmentioning

confidence: 99%

Functionality-type and chemical-composition separation for poly(lactide-co-glycolide) using gradient elution with basic and acidic additives in normal-phase liquid chromatography

Serizawa,

Reekers,

Delft

et al. 2024

Preprint

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The end groups of poly(lactide-co-glycolide) (PLGA) play a crucial role in determining the properties of polymers used in drug delivery systems. Research has shown that the encapsulation efficiency in PLGA microspheres can vary significantly between ester-terminated and acid-terminated PLGA. To study the functionality-type distribution (FTD) in PLGA polymers, researchers have used methods such as matrix-assisted laser desorption/ionization – high-resolution mass spectrometry and electrospray ionization – mass spectrometry. However, these methods are typically limited to PLGA polymers with a molecular weight of up to 4kDa. 13Carbon-nuclear-magnetic-resonance has also been used to differentiate and quantify PLGA end groups, but this method is time-consuming, taking over 12 hours per sample. To address these limitations, we have developed a normal-phase liquid chromatography method that can separate FTD and partial chemical composition distribution (CCD) in PLGA polymers. Our method can separate PLGA polymers with a molecular weight of up to 185 kDa and simultaneously separate the difference in lactic acid (LA)/glycolic acid (GA) ratios. To achieve this, we used a cross-linked diol column with a ternary gradient from hexane to 0.1% v/v triethylamine in THF to 0.1% v/v formic acid in THF. This allowed for the elution of ester-terminated PLGA, followed by acid-terminated PLGA. We also separated ester-terminated PLGA in the difference of the LA/GA ratio. Our method is expected to help understand the correlation between PLGA’s FTD, CCD, and physical properties, which will facilitate product development.

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Recycling gradient-elution liquid chromatography for the analysis of chemical-composition distributions of polymers

Cited by 8 publications

References 52 publications

Improvement of oligonucleotide separation using a repetto high‐performance liquid chromatography recycling approach

Improvement of oligonucleotide separation using a repetto high‐performance liquid chromatography recycling approach

The utilization of open‐source microcontroller boards and single‐board computers in liquid chromatography

Functionality-type and chemical-composition separation for poly(lactide-co-glycolide) using gradient elution with basic and acidic additives in normal-phase liquid chromatography

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