Topic Editors

School of Chemistry and Chemical Engineering, Guizhou University, Guiyang, China
School of Chemistry, Monash University, Caulfield East, VIC, Australia

Application of Liquid Chromatography-Mass Spectrometry and Related Techniques

Abstract submission deadline
15 October 2024
Manuscript submission deadline
15 December 2024
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Topic Information

Dear Colleagues,

The MDPI open access journals Analytica, Foods, Molecules, Sensors and Separations are combining to produce a special topic edition on “Application of Liquid Chromatography-Mass Spectrometry and Related Techniques”. All forms of liquid chromatography will be covered, including simple-column LC, HPLC, IC, TLC, SEC, etc. Although the main emphasis will be on LC–MS, it will also encompass related flow-based separation methods such as field-flow fractionation, hydrodynamic chromatography, etc., and it should be made clear that all forms of MS are included, e.g., ICP–MS, MS–MS.

Dr. Chao Kang
Dr. Ronald Beckett
Topic Editors

Participating Journals

Journal Name Impact Factor CiteScore Launched Year First Decision (median) APC
Analytica
analytica
- - 2020 15.6 Days CHF 1000 Submit
Foods
foods
5.2 5.8 2012 13.1 Days CHF 2900 Submit
Molecules
molecules
4.6 6.7 1996 14.6 Days CHF 2700 Submit
Sensors
sensors
3.9 6.8 2001 17 Days CHF 2600 Submit
Separations
separations
2.6 2.5 2014 13.6 Days CHF 2600 Submit

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Published Papers (11 papers)

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14 pages, 1953 KiB  
Article
Isolation and Identification of Bitter Compounds in Ginseng (Panax ginseng C. A. Mey.) Based on Preparative High Performance Liquid Chromatography, UPLC-Q-TOF/MS and Electronic Tongue
by Yang Chen, Ziwei Liao, Zhe Wang, Wanyin Shi and Jian Xu
Separations 2024, 11(4), 114; https://doi.org/10.3390/separations11040114 - 07 Apr 2024
Viewed by 285
Abstract
As a traditional Chinese medicinal herb, ginseng (Panax ginseng C. A. Mey.) is commonly used to treat common diseases, for example, esophageal cancer and myasthenia gravis. Furthermore, ginseng is also processed into a functional food additive that is utilized to improve the [...] Read more.
As a traditional Chinese medicinal herb, ginseng (Panax ginseng C. A. Mey.) is commonly used to treat common diseases, for example, esophageal cancer and myasthenia gravis. Furthermore, ginseng is also processed into a functional food additive that is utilized to improve the freshness of chicken soup and make health wine. Unfortunately, ginseng (Panax ginseng C. A. Mey.) has already shown a noticeable bitterness during its application process. In this research, the bitter substances in ginseng (Panax ginseng C. A. Mey.) after two common preparation processes (water extraction and ethanol extraction) were separated, purified and identified by preparative high performance liquid chromatography (prep-HPLC), high performance liquid chromatography with diode array detector (HPLC-DAD), ultra-performance liquid chromatography coupled with high-resolution quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF/MS) and an electronic tongue. The results indicated that compared with the other four bitter compounds, the ginsenoside Rb1 had the highest bitterness value, followed by 20(S)-ginsenoside Rg2, ginsenoside Rg1, ginsenoside Rf and ginsenoside Rb3. Upon the evaluation of results to reduce the bitterness of ginseng extract, we found that the composite embedding system of chitosan adsorption in the ginseng carrageenan gel microsphere (K/MC/MCG) could effectively reduce the bitterness. Full article
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16 pages, 2242 KiB  
Article
High-Resolution Mass Spectrometry-Based Metabolomics for Increased Grape Juice Metabolite Coverage
by Sébastien Nicolas, Benjamin Bois, Kevin Billet, Rémy Romanet, Florian Bahut, Jenny Uhl, Philippe Schmitt-Kopplin and Régis D. Gougeon
Foods 2024, 13(1), 54; https://doi.org/10.3390/foods13010054 - 22 Dec 2023
Viewed by 1094
Abstract
The composition of the juice from grape berries is at the basis of the definition of technological ripeness before harvest, historically evaluated from global sugar and acid contents. If many studies have contributed to the identification of other primary and secondary metabolites in [...] Read more.
The composition of the juice from grape berries is at the basis of the definition of technological ripeness before harvest, historically evaluated from global sugar and acid contents. If many studies have contributed to the identification of other primary and secondary metabolites in whole berries, deepening knowledge about the chemical composition of the sole flesh of grape berries (i.e., without considering skins and seeds) at harvest is of primary interest when studying the enological potential of widespread grape varieties producing high-added-value wines. Here, we used non-targeted DI-FT-ICR-MS and RP-UHPLC-Q-ToF-MS analyses to explore the extent of metabolite coverage of up to 290 grape juices from four Vitis vinifera grape varieties, namely Chardonnay, Pinot noir, Meunier, and Aligoté, sampled at harvest from 91 vineyards in Europe and Argentina, over three successive vintages. SPE pretreatment of samples led to the identification of more than 4500 detected C,H,O,N,S-containing elemental compositions, likely associated with tens of thousands of distinct metabolites. We further revealed that a major part of this chemical diversity appears to be common to the different juices, as exemplified by Pinot noir and Chardonnay samples. However, it was possible to build significant models for the discrimination of Chardonnay from Pinot noir grape juices, and of Chardonnay from Aligoté grape juices, regardless of the geographical origin or the vintage. Therefore, this metabolomic approach opens access to a remarkable holistic molecular description of the instantaneous composition of such a biological matrix, which is the result of complex interplays among environmental, biochemical, and vine growing practices. Full article
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14 pages, 5644 KiB  
Article
Effect of Air Drying on the Metabolic Profile of Fresh Wild and Artificial Cordyceps sinensis
by Tao Wang, Chuyu Tang, Mengjun Xiao, Zhengfei Cao, Min He, Jianzhao Qi, Yuling Li and Xiuzhang Li
Foods 2024, 13(1), 48; https://doi.org/10.3390/foods13010048 - 21 Dec 2023
Viewed by 714
Abstract
Fresh and dried Cordyceps sinensis are widely used by the public for medicinal and health purposes. However, the differences between them have not been examined. In this study, fresh wild and artificial C. sinensis (WFC and AFC) were dried to obtain dried wild [...] Read more.
Fresh and dried Cordyceps sinensis are widely used by the public for medicinal and health purposes. However, the differences between them have not been examined. In this study, fresh wild and artificial C. sinensis (WFC and AFC) were dried to obtain dried wild and artificial C. sinensis (WDC and ADC). Non-targeted GC-MS was used to analyze the metabolic profile characteristics of the four groups of samples. The results showed that air drying significantly altered the composition and content of C. sinensis, mainly in the form of higher abundance of organic acids and derivatives and lower abundance of lipids and lipid-like molecules in fresh C. sinensis. Hierarchical cluster analysis (HCA) and quantitative analyses showed that air drying increased the abundance of Valine, Zinniol, Urocanate, Vulpinic acid, and Uridine 5’-diphosphate, and decreased Xanthotoxol, Vitexin-4-o-glucoside, Val-trp, and Wogonin. These differentially accumulated metabolites (DAMs) were also shown to be potential biomarkers for C. sinensis. KEGG enrichment analysis identified lysine biosynthesis as the most significantly enriched pathway. Annotation of these DAMs to lysine biosynthesis revealed that citrate cycle and pyruvate metabolism entered lysine biosynthesis via 2-oxohlutarate and Homocitrate, respectively, resulting in significant enrichment of L-saccharopine and L-lysine content was significantly higher. Alanine, aspartate, and Glutamate metabolism synthesized more L-aspartate to promote L-lysine synthesis. Thus, high levels of L-lysine result in lysine degradation and pymolysine, which are the most active metabolic pathways during the drying of fresh C. sinensis and indirectly lead to differences in metabolic profiles. Full article
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16 pages, 3797 KiB  
Article
Optimization of QuEChERS Method for Antibiotic Residue Analysis in Animal Foods via Response Surface Methodology
by Xiaoqiong Wu, Yun Lin, Xiang Zhang, Nan Ouyang and Ying Zhou
Separations 2023, 10(8), 459; https://doi.org/10.3390/separations10080459 - 21 Aug 2023
Cited by 1 | Viewed by 999
Abstract
The present study employed a modified QuEChERS method to systematically analyze the presence of fifteen quinolone and seven tetracycline antibiotic residues in local animal food. Additionally, a multi-level four-factor Box–Behnken design (BBD) within the framework of response surface methodology (RSM) was utilized to [...] Read more.
The present study employed a modified QuEChERS method to systematically analyze the presence of fifteen quinolone and seven tetracycline antibiotic residues in local animal food. Additionally, a multi-level four-factor Box–Behnken design (BBD) within the framework of response surface methodology (RSM) was utilized to evaluate the factors impacting the detection efficiency of the sample pretreatment procedure. Optimization was performed via Design Expert® 10.0.3, and the factors, including the volume of the acetonitrile, the addition of formic acid, the duration of the extraction, and the addition of EDTA, were combined with experimental design until an optimal solution was reached. Finally, the sample was tested via ultra-high performance liquid chromatography-quadrupole-linear ion trap mass spectrometry (UPLC/MS/MS) in both multiple reaction monitoring (MRM) and enhanced product ion (EPI) scan modes on a QTRAP® 5500 instrument (AB SCIEX instruments, Framingham, MA, USA). The overall average recoveries from actual samples fortified with 22 antibiotics at three levels ranged from 73.8% to 98.5% based on the use of matrix-fortified calibration, with variations ranging from 5.80 to 12.4% (n = 6). The limits of detection and quantification were 0.3 μg kg−1 and 1.0 μg kg−1, respectively. Lastly, the modified method was applied to practical sample analysis in the daily risk monitoring and assessment of food safety with satisfactory stability and robustness. Full article
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10 pages, 1964 KiB  
Article
Ultra-High-Performance Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry for Simultaneous Pesticide Analysis and Method Validation in Sweet Pepper
by Han Yeol Bang, Yong-Kyoung Kim, Hyoyoung Kim, Eun Joo Baek, Taewoong Na, Kyu Sang Sim and Ho Jin Kim
Molecules 2023, 28(14), 5589; https://doi.org/10.3390/molecules28145589 - 22 Jul 2023
Viewed by 975
Abstract
Pesticides effectively reduce the population of various pests that harm crops and increase productivity, but leave residues that adversely affect health and the environment. Here, a simultaneous multicomponent analysis method based on ultra-high-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UHPLC-QTOF-MS) pretreated by the [...] Read more.
Pesticides effectively reduce the population of various pests that harm crops and increase productivity, but leave residues that adversely affect health and the environment. Here, a simultaneous multicomponent analysis method based on ultra-high-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UHPLC-QTOF-MS) pretreated by the QuEChERS method was developed to control the maximum residual levels. Among the 140 pesticides with high frequency of detection in agricultural products in Gyeongnam region in Korea for 5 years, 12 pesticides with high detection frequency in sweet pepper were selected. The analytical method is validated, linearities are r2 > 0.999, limit of detection (LOD) ranges from 1.4 to 3.2 µg/kg, and limit of quantification (LOQ) ranges from 4.1 to 9.7 µg/kg, and the recovery rate was 81.7–99.7%. In addition, it was confirmed that a meaningful value of these parameters can be achieved by determining the measurement uncertainty. The results proved that parameters such as recovery rate and relative standard deviation of the analysis method were within international standards. Using the developed method, better and safer sweet peppers will be provided to consumers, and effective pesticide residue management will be possible by expanding to other agricultural products. Full article
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12 pages, 680 KiB  
Article
Validation of the Ultra-Performance Liquid Chromatography with Tandem Mass Spectrometry Method for Simultaneous Analysis of Eighteen Compounds in the Traditional Herbal Prescription, Sanjoin-Tang
by Chang-Seob Seo and Hyeun-Kyoo Shin
Separations 2023, 10(7), 411; https://doi.org/10.3390/separations10070411 - 18 Jul 2023
Cited by 1 | Viewed by 723
Abstract
Sanjoin-tang (SJIT) is an ancient oriental medicine prescription listed in the Jinguiyaolue that is mainly used for the treatment of primary insomnia. This study was conducted to develop and validate an ultra-performance liquid chromatography with tandem mass spectrometry (UPLC–MS/MS) simultaneous analysis method for [...] Read more.
Sanjoin-tang (SJIT) is an ancient oriental medicine prescription listed in the Jinguiyaolue that is mainly used for the treatment of primary insomnia. This study was conducted to develop and validate an ultra-performance liquid chromatography with tandem mass spectrometry (UPLC–MS/MS) simultaneous analysis method for the quality control of SJIT using 18 target compounds. The 18 analytes were separated on an Acquity UPLC BEH C18 column maintained at 45 °C using a mobile phase composed of distilled water and acetonitrile. The MS system was used to simultaneously detect all analytes using the multiple reaction monitoring (MRM) method of Xevo TQ-XS coupled with an electrospray ionization source. The concentrations of the 18 analytes investigated in the SJIT samples ranged from below the limit of detection to 9.553 mg/g. In conclusion, the validated UPLC–MS/MS MRM analysis method can be used to obtain basic data to establish chemical-nonclinical linkage efficacy and for the clinical research and quality evaluation of SJIT. Full article
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11 pages, 2460 KiB  
Article
The Residue and Dietary Risk Assessment of Spirotetramat and Its Four Metabolites in Cabbage Using Ultra-High-Performance Liquid Chromatography–Tandem Mass Spectrometry
by Junli Cao, Jindong Li, Pengcheng Ren, Yanli Qi and Shu Qin
Molecules 2023, 28(12), 4763; https://doi.org/10.3390/molecules28124763 - 14 Jun 2023
Viewed by 994
Abstract
Spirotetramat is a potential tetronic acid pesticide for controlling various pests with piercing–sucking mouthparts. To clarify its dietary risk on cabbage, we established an ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method and then investigated the residual levels of spirotetramat and its four metabolites [...] Read more.
Spirotetramat is a potential tetronic acid pesticide for controlling various pests with piercing–sucking mouthparts. To clarify its dietary risk on cabbage, we established an ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method and then investigated the residual levels of spirotetramat and its four metabolites in cabbage collected from field experiments under good agricultural practices (GAPs). The average recoveries of spirotetramat and its metabolites in cabbage were 74~110%, while the relative standard deviation (RSD) was 1~6%, and the limit of quantitation (LOQ) was 0.01 mg kg−1. The terminal residue of spirotetramat was in the range of <0.05~0.33 mg kg−1, the chronic dietary risk (RQc) was 17.56%, and the acute dietary risk (RQa) was 0.025~0.049%, which means an acceptable dietary intake risk. This study provides data to guide on the use of spirotetramat and to establish the maximum residue limits (MRLs) of spirotetramat on cabbage. Full article
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18 pages, 3484 KiB  
Article
Changes in the VOC of Fruits at Different Refrigeration Stages of ‘Ruixue’ and the Participation of Carboxylesterase MdCXE20 in the Catabolism of Volatile Esters
by Dongmei Li, Jianhua Guo, Hai Ma, Linna Pei, Xiaojie Liu, Hui Wang, Rongxin Chen, Zhengyang Zhao and Hua Gao
Foods 2023, 12(10), 1977; https://doi.org/10.3390/foods12101977 - 12 May 2023
Cited by 2 | Viewed by 1559
Abstract
Aroma is a crucial quality attribute of apple fruit, which significantly impacts its commercial value and consumer choice. Despite its importance the volatile aroma substances produced by the new variety ‘Ruixue’ after harvest remain unclear. In this study, we utilized headspace solid phase [...] Read more.
Aroma is a crucial quality attribute of apple fruit, which significantly impacts its commercial value and consumer choice. Despite its importance the volatile aroma substances produced by the new variety ‘Ruixue’ after harvest remain unclear. In this study, we utilized headspace solid phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) to investigate the changes in volatile substances, fruit hardness, crispness, and related aroma synthase activity of commercially mature ‘Ruixue’ apples during cold storage. Our findings revealed a gradual decline in fruit firmness and brittleness of ‘Ruixue’ apples during cold storage, with hexyl acetate, hexyl caproate, and hexyl thiocyanate being the main hexyl esters detected. To gain a better understanding of the metabolic pathway of esters, we identified 42 MdCXE gene members that are associated with ester degradation. Through RT-qPCR analysis, we discovered that carboxylesterase MdCXE20 exhibited higher expression levels compared to other MdCXE genes during cold storage. To confirm the role of MdCXE20, we conducted a transient injection of apple fruits and observed that overexpression of MdCXE20 led to the degradation of esters such as hexyl hexanoate, butyl hexanoate, butyl 2-methylbutyrate, hexyl butyrate, and hexyl 2-methylbutyrate. The results of the study showed that the virus-induced gene silencing of MdCXE20 found the opposite results. Additionally, the esters of OE-MdCXE20 callus showed a lower content of ester VOC than the control callus, according to the homologous stable transformation of ‘Wanglin’ callus. Overall, these findings suggest that the MdCXE20 gene plays a crucial role in the decrease of esters in ‘Ruixue’ apples, which ultimately affects their flavor. Full article
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11 pages, 855 KiB  
Communication
Simultaneous Analysis of Bergapten and Schinifoline in Zanthoxylum schinifolium Seeds Using HPLC and UPLC-MS/MS Systems
by Chang-Seob Seo
Foods 2023, 12(7), 1355; https://doi.org/10.3390/foods12071355 - 23 Mar 2023
Viewed by 1098
Abstract
Zanthoxylum schinifolium Siebold et Zuccarini belongs to the Rutaceae family and has been widely used as a spice in East Asian countries such as Korea, China, and Japan. The present study focused on developing and validating a simultaneous analytical method for marker substances [...] Read more.
Zanthoxylum schinifolium Siebold et Zuccarini belongs to the Rutaceae family and has been widely used as a spice in East Asian countries such as Korea, China, and Japan. The present study focused on developing and validating a simultaneous analytical method for marker substances (bergapten and schinifoline) in Z. schinifolium seeds. This was achieved using high-performance liquid chromatography with a photo-diode array detector (HPLC-PDA) and ultra-performance liquid chromatography with tandem mass spectrometry (UPLC-MS/MS) systems. In the regression equation, all markers showed a coefficient of determination of ≥0.9990. Marker recovery was 96.90–105.16% (relative standard deviation (RSD) ≤ 2.23), and the intra- and interday precision was RSD < 3.00. Bergapten and schinifoline were detected in the seeds at 1.70–2.85 mg/g and 0.19–0.94 mg/g, respectively. This analytical method will improve quality control of Z. schinifolium seeds. Additionally, this assay will provide basic data and quality assurance for future biological activity experiments or clinical applications. Full article
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15 pages, 2037 KiB  
Article
Simultaneous Determination of Neonicotinoid and Carbamate Pesticides in Freeze-Dried Cabbage by Modified QuEChERS and Ultra-Performance Liquid Chromatography–Tandem Mass Spectrometry
by Bingxin Yang, Sheng Wang, Wen Ma, Guanlin Li, Mengling Tu, Zhiyong Ma, Qinghe Zhang, Hongmei Li and Xianjiang Li
Foods 2023, 12(4), 699; https://doi.org/10.3390/foods12040699 - 06 Feb 2023
Cited by 8 | Viewed by 1590
Abstract
Dehydrated vegetables are popular in instant foods, but few reports have focused on their pesticide residues. This research developed and validated a modified QuEChERS method combined with ultra-performance liquid chromatography–tandem mass spectrometry to determine 19 kinds of neonicotinoid and carbamate pesticides in freeze-dried [...] Read more.
Dehydrated vegetables are popular in instant foods, but few reports have focused on their pesticide residues. This research developed and validated a modified QuEChERS method combined with ultra-performance liquid chromatography–tandem mass spectrometry to determine 19 kinds of neonicotinoid and carbamate pesticides in freeze-dried cabbage. Herein, acetonitrile/water (v/v = 2:1) was selected in the extraction step. Meanwhile, 4 g anhydrous magnesium sulfate and 1 g sodium chloride were applied to the partitioning step. Dispersive solid-phase extraction sorbents were selected, and liquid chromatography conditions were further optimized for dealing with the matrix effect. The limits of quantification ranged from 1.0 to 10.0 μg/kg. The validation results were acceptable, with average recoveries of 78.7–114.0% and relative standard deviations below 14.2%. The method recoveries were closely related to the volume proportion of water in the extractant. Finally, the developed method was applied to real freeze-dried cabbages and four pesticides (propamocarb, imidacloprid, acetamiprid, and thiacloprid) were detected in six samples. Full article
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15 pages, 1085 KiB  
Article
Analysis of Chemical Constituents of Traditional Chinese Medicine Jianqu before and after Fermentation Based on LC-MS/MS
by Yishuo Wang, Ruisheng Wang, Zhenling Zhang, Yitian Chen, Mengmei Sun, Jia Qiao and Ziwei Du
Molecules 2023, 28(1), 53; https://doi.org/10.3390/molecules28010053 - 21 Dec 2022
Cited by 2 | Viewed by 1868
Abstract
Objective: To detect the chemical constituents in Jianqu samples under different fermentated states by using UPLC-QTOF-MS/MS technology, to conduct preliminary analyses, and to establish an HPLC method for the simultaneous determination of hesperidin and naringenin in Jianqu, and the variation of the two [...] Read more.
Objective: To detect the chemical constituents in Jianqu samples under different fermentated states by using UPLC-QTOF-MS/MS technology, to conduct preliminary analyses, and to establish an HPLC method for the simultaneous determination of hesperidin and naringenin in Jianqu, and the variation of the two components during fermentation were compared. Methods: Waters ACQUITYTM UPLC HSST3 column (2.1 mm × 100 mm, 1.8 μm) was used; the mobile phase was 0.1% formic acid aqueous solution (A)-0.1% formic acid acetonitrile (B); The flow rate was 0.4 mL·min−1 with gradient elution; the column temperature was 45 °C; injection volume was 5 μL. The mass spectra of the samples were collected by negative ion mode under the electrospray ion source, and the data were screened and matched by UNIFI software. Hypersil gold C18 column (100 mm × 2.1 mm, 1.9 μm) was used; the mobile phase was acetonitrile (A)-0.1% acetic acid (B);; the flow rate with gradient elution was 0.3 mL·min−1; the column temperature was 30 °C; the injection volume was 2 μL. The content changes of hesperetin and naringenin in Jianqu at different fermentation time were detected. Results: A total of 54 compounds were identified, including flavonoids, amino acids, organic acids, terpenoids, coumarins, lignans, and other compounds. Under the selected HPLC conditions, the linear relationship between hesperidin and naringenin was discovered (r2 = 0.9996). The content of hesperidin and naringenin changed significantly in the whole fermentation process. The highest concentration of content was observed at 36 h of fermentation and then decreased to varying degrees. Conclusion: This experiment can effectively identify various chemical components in Jianqu during different fermentation periods, and determine the content of the characteristic components, so as to provide a scientific basis for further study of Jianqu fermentation processing technology as well as a sound pharmacodynamic material basis. Full article
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