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Chromatography-Mass Spectrometry Technology Research
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Chromatography-Mass Spectrometry Technology Research

A special issue of Separations (ISSN 2297-8739). This special issue belongs to the section "Chromatographic Separations".

Deadline for manuscript submissions: closed (31 May 2023) | Viewed by 18042

Special Issue Editors

Dr. Tomasz Śniegocki

E-Mail Website
Guest Editor
Department of Pharmacology and Toxicology, National Veterinary Research Institute, Pulawy, Poland
Interests: food safety; gas chromatography; liquid chromatography; mass spectrometry; method development and validation; sample preparation
Dr. Jakub Trawiński

E-Mail Website
Guest Editor
Department of Medicinal Chemistry, Medical University of Lublin, Lublin, Poland
Interests: bioanalysis; pharmaceutical analysis; environmental pollution; pesticides residues; metabolites; xenobiotics; food analysis; sample preparation; liquid chromatography–mass spectrometry

Special Issue Information

Dear Colleagues,

This Special Issue, “Chromatography-Mass Spectrometry Technology Research”, aims to present new methods or news technique for the detection and quantification of various xenobiotics in different matrices. 

Mass spectrometry is an analytical technique that allows the precise measurement of the mass to electric charge ratio of an ion, where with a known charge of the ion, it is possible to calculate the mass with the accuracy of single atoms. The combination of chromatography and mass spectrometry is a powerful tool for the determination of different compounds or their groups in biological samples, in pharmacokinetic studies, and also the identification and monitoring of contaminants in food or environmental matrices. Additionally, it is an important tool not only in the detection and determination of parent compounds but also their metabolites.

Therefore, it is our pleasure to invite you to contribute your research articles or communications to this Special Issue dedicated to new methods or techniques applied for the detection and quantification of various xenobiotics and/or their metabolites in different matrices. We believe that your contribution to this Special Issue will definitely have a significant impact on the entire scientific research community.

Thank you for your kind consideration.

Dr. Tomasz Śniegocki
Dr. Jakub Trawiński
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Separations is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2600 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • bioanalysis
  • pharmaceutical analysis
  • environmental pollution
  • pesticides residues
  • metabolites
  • xenobiotics
  • food analysis
  • contaminants
  • sample preparation
  • liquid chromatography-mass spectrometry

Published Papers (10 papers)

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Research

11 pages, 1185 KiB  
Article
Pharmacokinetics of Lixisenatide, a GLP-1 Receptor Agonist, Determined by a Novel Liquid Chromatography–Tandem Mass Spectrometry Analysis in Rats
by Hyeon Seok Oh, Eun Ji Park, Tae Suk Lee, Yejin An, Tae Hwan Kim, Soyoung Shin and Beom Soo Shin
Separations 2023, 10(5), 282; https://doi.org/10.3390/separations10050282 - 26 Apr 2023
Cited by 1 | Viewed by 2137
Abstract
Because of its greater binding affinity and longer half-life than native glucagon-like peptide-1 (GLP-1), the GLP-1 receptor agonist lixisenatide is commonly used to treat type 2 diabetes mellitus. This study aimed to establish a simple and robust liquid chromatography–tandem mass spectrometry (LC–MS/MS) approach [...] Read more.
Because of its greater binding affinity and longer half-life than native glucagon-like peptide-1 (GLP-1), the GLP-1 receptor agonist lixisenatide is commonly used to treat type 2 diabetes mellitus. This study aimed to establish a simple and robust liquid chromatography–tandem mass spectrometry (LC–MS/MS) approach for lixisenatide for in vivo pharmacokinetic investigation. Methanol-based protein precipitation with formic acid was exploited for plasma sample extraction, using esomeprazole as the internal standard. Gradient elution with 0.1% formic acid in distilled water and acetonitrile was utilized for chromatographic separation. Mass spectrometry was used to monitor the MRM transition at m/z 810.8 → 129.2 for lixisenatide. In rat plasma, lixisenatide had a lower limit of quantification of 10 ng/mL. The LC–MS/MS was applied to describe the pharmacokinetics of lixisenatide in rats following intravenous and subcutaneous dosing. The average half-life of lixisenatide was 0.37 ± 0.06 h after intravenous injection. The estimated subcutaneous bioavailability of lixisenatide was 2.17%. This LC–MS/MS analysis might be relevant in future research to create novel dosage formulations of lixisenatide and other GLP-1 receptor agonists with optimal therapeutic effectiveness. Full article
(This article belongs to the Special Issue Chromatography-Mass Spectrometry Technology Research)
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16 pages, 4368 KiB  
Article
Evaluating the Degradation Process of Collagen Sponge and Acellular Matrix Implants In Vivo Using the Standardized HPLC-MS/MS Method
by Jianping Gao, Ye Ma, Zhenhu Guo, Yang Zhang, Fangyu Xing, Tianyang Zhang, Yingjun Kong, Xi Luo, Liming Xu and Guifeng Zhang
Separations 2023, 10(1), 47; https://doi.org/10.3390/separations10010047 - 12 Jan 2023
Cited by 3 | Viewed by 2098
Abstract
The purpose of this study was to establish a collagen determination method based on an isotope-labeled collagen peptide as an internal reference via high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS), and using the established method to evaluate the degradation process of collagen-based implants in [...] Read more.
The purpose of this study was to establish a collagen determination method based on an isotope-labeled collagen peptide as an internal reference via high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS/MS), and using the established method to evaluate the degradation process of collagen-based implants in vivo. The specific peptide (GPAGPQGPR) of bovine type I collagen was identified with an Orbitrap mass spectrometer. Then, the quantification method based on the peptide detection with HPLC-MS/MS was established and validated, and then further used to analyze the degradation trend of the collagen sponge and acellular matrix (ACM) in vivo at 2, 4, 6, 8, 12, 16, and 18 weeks after implantation. The results indicate that the relative standard deviation (RSD) of the detection precision and repeatability of the peptide-based HPLC-MS/MS quantification method were 3.55% and 0.63%, respectively. The limitations of quantification and detection were 2.05 × 10−3 μg/mL and 1.12 × 10−3 μg/mL, respectively. The collagen sponge and ACM were completely degraded at 10 weeks and 18 weeks, respectively. Conclusion: A specific peptide (GPAGPQGPR) of bovine type I collagen was identified with an Orbitrap mass spectrometer, and a standardized HPLC-MS/MS-based internal reference method for the quantification of bovine type I collagen was established. The method can be used for the analysis of the degradation of collagen-based implants in vivo. Full article
(This article belongs to the Special Issue Chromatography-Mass Spectrometry Technology Research)
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10 pages, 2006 KiB  
Article
A Natural Monoterpene Enol for Dispersive Liquid–Liquid Microextraction Based on Solidification of Floating Organic Droplets for Determination of Benzophenone Compounds in Water Samples
by Xian Zhang, Luyun Zhang, Dan Zheng, Zhenzhen Xia, Maomin Peng, Danling Sun, Xizhou Hu and Xitian Peng
Separations 2023, 10(1), 1; https://doi.org/10.3390/separations10010001 - 20 Dec 2022
Cited by 3 | Viewed by 1251
Abstract
In the current study, an effective and simple procedure of extraction for the four benzophenone compounds from water samples was achieved by dispersive liquid–liquid microextraction (DLLME) based on the solidification of floating organic droplets (SFO) with a natural monoterpene enol as the extractant. [...] Read more.
In the current study, an effective and simple procedure of extraction for the four benzophenone compounds from water samples was achieved by dispersive liquid–liquid microextraction (DLLME) based on the solidification of floating organic droplets (SFO) with a natural monoterpene enol as the extractant. As a natural, high solidification point, inexpensive, and environmentally friendly hydrophobic solvent, α−terpineol was selected firstly as an extractant for DLLME and could be collected and transferred easily after extraction by solidification at a lower temperature. Several main parameters closely related to extraction efficiencies, such as volume of extractant, extraction time, pH and salt concentration of the sample solution, temperature, and time of the solidification process, were investigated in detail. The results showed that the established method had good extraction performance for benzophenone compounds with enrichment factors in the range of 29–47. Furthermore, the linearities were over the range of 2–2000 µg/L, and the limits of detection were 0.12–0.53 µg/L for four benzophenone compounds. The recoveries ranged from 80.2% to 108.4%, with RSDs (intra- and inter-assay) less than 8.5%. At last, the method applicability was investigated by the determination of the benzophenone compounds in aqueous solutions, and satisfactory recoveries (83.0–107.0%) were acquired. Taken together, α−terpineol, a natural monoterpene enol, was first used as an extractant of DLLME-SFO, which provided an alternative method with simplicity and rapidity for the determination of benzophenone compounds in aqueous samples. Full article
(This article belongs to the Special Issue Chromatography-Mass Spectrometry Technology Research)
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15 pages, 2475 KiB  
Article
Purification of Two Taxanes from Taxus cuspidata by Preparative High-Performance Liquid Chromatography
by Yajing Zhang, Zirui Zhao, Wenlong Li, Yuanhu Tang, Huiwen Meng and Shujie Wang
Separations 2022, 9(12), 446; https://doi.org/10.3390/separations9120446 - 16 Dec 2022
Cited by 1 | Viewed by 1645
Abstract
In the present study, an effective method of preparative high-performance liquid chromatography (Prep-HPLC) was established to purify two taxanes in Taxus cuspidata. During the experimental operation, the effects of flow rate, injection volume, and column temperature on the purity of 10-deacetyltaxol (10-DAT) [...] Read more.
In the present study, an effective method of preparative high-performance liquid chromatography (Prep-HPLC) was established to purify two taxanes in Taxus cuspidata. During the experimental operation, the effects of flow rate, injection volume, and column temperature on the purity of 10-deacetyltaxol (10-DAT) and paclitaxel (PTX) were investigated, and the optimized conditions were as follows: flow rate of 10 mL/min, injection volume of 0.5 mL, and column temperature of 30 °C. Under these conditions, the purity of 10-DAT and PTX reached 95.33% and 99.15%, respectively. The purified products were characterized by scanning electron microscopy (SEM), high-performance liquid chromatography (HPLC), and electrospray ionization-high resolution mass spectrometry (ESI-HRMS). The results demonstrated that preparative HPLC can effectively purify 10-DAT and PTX from Taxus cuspidata with a purity of >95%, which was suitable for the large-scale preparation of 10-DAT and PTX. Full article
(This article belongs to the Special Issue Chromatography-Mass Spectrometry Technology Research)
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14 pages, 4384 KiB  
Article
Comprehensive Controller for Super Sonic Molecular Beam Gas Chromatograph Mass Spectrometer
by Eli Flaxer
Separations 2022, 9(12), 417; https://doi.org/10.3390/separations9120417 - 07 Dec 2022
Viewed by 1089
Abstract
This paper presents a new, comprehensive digital circuit used for the control of a novel gas chromatograph mass spectrometer (GC-MS) interface that is based on supersonic molecular beam (SMB). The circuit includes a Texas Instruments 150 MHz digital signal controller (DSC), high voltage [...] Read more.
This paper presents a new, comprehensive digital circuit used for the control of a novel gas chromatograph mass spectrometer (GC-MS) interface that is based on supersonic molecular beam (SMB). The circuit includes a Texas Instruments 150 MHz digital signal controller (DSC), high voltage amplifiers for 8 independent channels and 4 independent channels of high resolution pulse width modulation (PWM). The circuit, along with a sophisticated embedded program and a custom made personal computer (PC) application, control all aspects of the interface: smart filament emission-current stabilization, static and scanning mass-dependent ion-source voltages, transfer-line heater proportional integral differential (PID) controls with thermocouple feedbacks, on/off valves, relays and several peripheral device controls that enable the full operation of a turbo-molecular vacuum pump, and of gas flow and pressure controllers. All aspects of this comprehensive controller were successfully tested. The signal for the 450 Th ion (C32H66) for example increased by 123% which is a significant increase. It is obvious that correctly tuned dynamic voltages can guarantee the optimal signal for each mass. Full article
(This article belongs to the Special Issue Chromatography-Mass Spectrometry Technology Research)
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16 pages, 4552 KiB  
Article
Metabolite Profiling of Tartary Buckwheat Extracts in Rats Following Co-Administration of Ethanol Using UFLC-Q-Orbitrap High-Resolution Mass Spectrometry
by Liping Xiang, Jian Xu, Wanyu Liu, Yue Wu, Xin Jiang, Yixin Hu, Yao Zhang, Qiang Yang, Zhe Wang, Yuejun Yang, Sanlan Wu, Luqin Si, Jiangeng Huang and Yongjun Zhang
Separations 2022, 9(12), 407; https://doi.org/10.3390/separations9120407 - 02 Dec 2022
Viewed by 1106
Abstract
Tartary buckwheat, a gluten-free pseudocereal, has received considerable attention owing to its unique nutritional ingredients and beneficial health effects such as anti-tumor, anti-oxidation, anti-inflammation and hepatoprotective activities. Pharmacokinetic and metabolite profiling have been preliminarily assessed for Tartary buckwheat extracts. However, its metabolites have [...] Read more.
Tartary buckwheat, a gluten-free pseudocereal, has received considerable attention owing to its unique nutritional ingredients and beneficial health effects such as anti-tumor, anti-oxidation, anti-inflammation and hepatoprotective activities. Pharmacokinetic and metabolite profiling have been preliminarily assessed for Tartary buckwheat extracts. However, its metabolites have not yet been characterized in vivo after co-administration with ethanol when Tartary buckwheat extracts are used for the treatment of alcoholic liver disease. In this paper, a Q-Exactive orbitrap high-resolution mass spectrometer was employed to identify the metabolites of Tartary buckwheat extracts in rat biological samples. Compared with previous metabolite profiling results, a total of 26 novel metabolites were found in rat biological samples, including 11, 10, 2 and 5 novel metabolites in rat plasma, bile, urine and feces, respectively, after oral co-administration of 240 mg/kg Tartary buckwheat extracts with ethanol (42%, v/v). The major metabolic pathways of the constituents in Tartary buckwheat extracts involved hydroxylation, methylation, glucuronidation, acetylation and sulfation. Quercetin and its metabolites may be the pharmacological material basis of Tartary buckwheat for the protective effect against alcoholic liver injury. The research enriched in vivo metabolite profiling of Tartary buckwheat extracts, which provided experimental data for a comprehensive understanding and rational use of Tartary buckwheat against alcoholic liver disease. Full article
(This article belongs to the Special Issue Chromatography-Mass Spectrometry Technology Research)
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10 pages, 1807 KiB  
Article
Residual Characteristics of Atrazine and Its Metabolites in the Liaoning Province of China
by Wei Meng, Daifeng Wang, Shizhong Li, Yuying Wang, Ce Jiang, Hongzhe Tian and Mingshan Ji
Separations 2022, 9(12), 397; https://doi.org/10.3390/separations9120397 - 28 Nov 2022
Cited by 3 | Viewed by 1372
Abstract
The simultaneous determination of atrazine residue and its metabolites was developed using liquid chromatography-tandem mass spectrometry in Liaoning Province, China. To ensure agricultural production and environmental safety, their contamination level was assessed. A total of 2142 samples were collected between 2014 and 2020, [...] Read more.
The simultaneous determination of atrazine residue and its metabolites was developed using liquid chromatography-tandem mass spectrometry in Liaoning Province, China. To ensure agricultural production and environmental safety, their contamination level was assessed. A total of 2142 samples were collected between 2014 and 2020, including 1213 soil samples, 190 surface water samples, and 739 groundwater samples. The overall pollution level and detectable level of the herbicides in Liaoning Province was found to be the highest in soil followed by surface water and groundwater. The residual level of the analytes in the collected samples decreased in the following order: atrazine > hydroxyatrazine > desethylatrazine > desisopropylatrazine. From 2014 to 2020, atrazine was detected in soil and surface water, whereas hydroxyatrazine was found in soil without the selected analytes detected in groundwater. The pollution of atrazine in soil was higher than that of hydroxyatrazine, desethylatrazine, and desisopropylatrazine. To maintain sustainable agricultural development, it is critical to pay attention to the residual determination of atrazine in the environment. Full article
(This article belongs to the Special Issue Chromatography-Mass Spectrometry Technology Research)
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11 pages, 1403 KiB  
Article
Rapid Determination of Metribuzin and Three Major Transformation Products in Soil and Plant by Gas Chromatography–Tandem Mass Spectrometry
by Beatriz Albero, María Dolores Fernández, Concepción García-Gómez and Rosa Ana Pérez
Separations 2022, 9(12), 386; https://doi.org/10.3390/separations9120386 - 23 Nov 2022
Cited by 2 | Viewed by 1905
Abstract
Metribuzin is a pre- and post-emergence triazinone herbicide used in a variety of crops. This herbicide is degraded in the environment into three major metabolites that have high water solubility, high to very high soil mobility, and low to moderate persistence in soil. [...] Read more.
Metribuzin is a pre- and post-emergence triazinone herbicide used in a variety of crops. This herbicide is degraded in the environment into three major metabolites that have high water solubility, high to very high soil mobility, and low to moderate persistence in soil. This paper describes the development of an analytical method based on ultrasound-assisted extraction and GC-MS/MS determination for the determination metribuzin and its main metabolites in soil and plants. The developed method provided good recoveries for all compounds in soil and plants (from 73 to 121%). The quantitation limits obtained from plants (2.6 to 18 µg/kg) allow determining the presence of these compounds at trace levels. To evaluate the applicability of the developed methods, bean plants were grown in plastic pots with soil treated with metribuzin and collected after 23 days. At the end of the assay, only 11% of the initial concentration of metribuzin remained in soil. Metribuzin and its three metabolites were detected in plants, desamino-diketo-metribuzin is the most abundant metabolite. It is expected that the application of these methods can provide more data to monitor metribuzin residues due to herbicide treatments. Full article
(This article belongs to the Special Issue Chromatography-Mass Spectrometry Technology Research)
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15 pages, 2917 KiB  
Article
Development of Analytical Procedure for the Determination of 17β-Testosterone, 11-Ketotestosterone and 17β-Estradiol in the Sea Trout (Salmo trutta L.) Gonads
by Iwona Matraszek-Żuchowska, Alicja Kłopot, Sebastian Witek, Agnieszka Pękala-Safińska and Andrzej Posyniak
Separations 2022, 9(10), 293; https://doi.org/10.3390/separations9100293 - 06 Oct 2022
Cited by 1 | Viewed by 1282
Abstract
Steroid hormones, such as 17β-testosterone, 11-ketotestorenone and 17β-estradiol, play an essential role not only in reproductive function but also are potential biomarkers of numerous additional functions in teleost fish. The presence of endocrine disruptor compounds in aquatic ecosystems has raised concern about their [...] Read more.
Steroid hormones, such as 17β-testosterone, 11-ketotestorenone and 17β-estradiol, play an essential role not only in reproductive function but also are potential biomarkers of numerous additional functions in teleost fish. The presence of endocrine disruptor compounds in aquatic ecosystems has raised concern about their effect on hormone levels in fish target organs. Since hormones are present in very low concentrations in biological material, their determination still remains a challenge. A new analytical procedure has been developed to determine 17β-testosterone, 11-ketotestosterone and 17β-estradiol in the sea trout female and male gonads by liquid chromatography-tandem mass spectrometry (LC-MS/MS) system equipped with an ESI source operating in both positive and negative mode. Chromatographic separation of analytes was accomplished in Poroshell 120 EC-C18 (150 mm × 2.1 mm, 2.7 µm) column under isocratic elution conditions. The mobile phase consisted of acetonitrile, methanol and water (20:50:30/v/v/v) at a flow rate of 0.2 mL/min. Analytes were extracted from the gonad matrix with ethyl acetate, and co-extractives impurities were successfully removed by QuEChERS (quick, easy, cheap, effective, rugged and safe) method. The procedure was validated with good sensitivity, linearity, accuracy, and precision. Limits of quantifications were from 0.15 to 0.75 ng/g, linearity was obtained with correlation coefficient R > 0.99, accuracy was from 94.0 to 109.5%, precision expressed as RSD ranged from 1.7 to 27.2% (repeatability) and from 2.2 to 37.1% (reproducibility). Finally, the method was applied to determining 17β-testosterone, 11-ketotestosterone and 17β-estradiol in real samples of the female and male sea trout gonads, 8 and 22 samples, respectively. Full article
(This article belongs to the Special Issue Chromatography-Mass Spectrometry Technology Research)
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10 pages, 2730 KiB  
Article
Influence and Mechanism of Polar Solvents on the Retention Time of Short-Chain Fatty Acids in Gas Chromatography
by Mu Ren, Narantsogt Natsagdorj and Na Shun
Separations 2022, 9(5), 124; https://doi.org/10.3390/separations9050124 - 16 May 2022
Cited by 3 | Viewed by 3114
Abstract
Short-chain fatty acids (SCFAs), produced by microbes when dietary fiber ferments in the colon, are one of the most studied microbial products despite their volatility and complex matrices, which make analysis challenging. In the current study, we sought to address research gaps by [...] Read more.
Short-chain fatty acids (SCFAs), produced by microbes when dietary fiber ferments in the colon, are one of the most studied microbial products despite their volatility and complex matrices, which make analysis challenging. In the current study, we sought to address research gaps by exploring the commonalities and differences between the retention time changes for SCFAs in polar solvents. In one such solvent, dimethyl sulfoxide (DMSO), the retention time of the SCFA acetic acid shows a linear positive correlation with the equal volume increase in the DMSO solvent. We used gas chromatography–mass spectrometry to analyze the retention times of mixed solutions of formic acid, acetic acid, butyric acid, valeric acid, and toluene in the solvents DMSO and water and found that only the retention times of formic acid and acetic acid changed. We further compared the effect of three solvents with similar polarities, DMSO, N-methylpyrrolidone (NMP), and dimethylformamide (DMF), on the retention time of acetic acid and found that it increased in the DMSO–water solution more than in the NMP–water solution and remained unchanged in the DMF–water solution. This finding is consistent with quantum chemical calculations showing that the strength of the hydrogen bond between DMSO and acetic acid is greater than between NMP and acetic acid. Taken together, the chromatographic results and quantum chemical calculations indicate that, in all three solvents, the portion of the molecule with the smallest negative electrostatic potential (red) has high electron density and can easily donate electrons, forming a hydrogen bond with acetic acid. However, the portion with the largest positive electrostatic potential (blue) forms a bond with polyethylene glycol, a column stationary solution with a strong dipole moment, and is adsorbed on the stationary solution in the direction of the dipole moment. Therefore, the retention times of formic acid and acetic acid change under the combined influence of a series of complex intermolecular forces. In the chromatographic column, the outflow rate of DMF is higher than that of acetic acid, and the force of the hydrogen bond between DMF and acetic acid cannot overcome the outflow resistance of acetic acid, so the retention time of the acetic acid in the DMF–water solution does not change. The retention times of butyric acid and valeric acid are unchanged in aprotic polar solvents for the same reason. Full article
(This article belongs to the Special Issue Chromatography-Mass Spectrometry Technology Research)
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