Article
Chemistry, Analytical
Troy T. Handlovic, M. Farooq Wahab, Daniel W. Armstrong
Summary: This paper presents an algorithm for peak symmetrization, addressing the issue of peak asymmetry in chiral analysis. The algorithm involves adding the correct fraction of the first derivative to the chromatogram to symmetrize raw chromatographic data. The paper also provides methods for extracting the distortion parameter and suppressing high frequencies using the perfect smoother algorithm. Additionally, a survey of 40 chiral separations is presented, demonstrating the range of asymmetry observed, along with examples of symmetrization of enantiomer peaks in comparable and disproportionate concentrations.
ANALYTICAL CHEMISTRY
(2022)
Article
Chemistry, Analytical
Yandi Fu, Francesc Borrull, Rosa Maria Marce, Naria Fontanals
Summary: This review discusses the determination and analysis of enantiomeric fractions of chiral drugs in environmental matrices using chiral liquid chromatography coupled with mass spectrometry. It provides a comprehensive overview and comparison of various techniques, addresses advancements and limitations, and explores the impact of the mobile phase composition on enantioseparation and MS detection. Various applications of chiral LC and MS for enantiomeric fraction determination of chiral drugs in environmental samples are also discussed in depth.
TRENDS IN ENVIRONMENTAL ANALYTICAL CHEMISTRY
(2021)
Article
Chemistry, Analytical
Maider Greno, Maria Luisa Marina, Maria Castro-Puyana
Summary: Two electrokinetic chromatography methods for the stereoselective determination of cysteine were developed and validated in this work, using different chiral selectors. Good enantiomeric resolutions were achieved in a short analysis time, with successful quantitation of cysteine in dietary supplements.
MICROCHEMICAL JOURNAL
(2021)
Review
Biochemistry & Molecular Biology
Robert Berkecz, Gabor Nemeti, Antal Peter, Istvan Ilisz
Summary: Chiral compounds play a crucial role in living organisms, making the enantioseparation of compounds a key task in modern analytical chemistry. High-performance liquid chromatography is the most commonly used method for separating chiral compounds.
Article
Chemistry, Multidisciplinary
Shirong Cao, Qianyun Ma, Ye Liu, Jiayu Zhang, Zhaokun Wang
Summary: In this study, direct chiral separation of ofloxacin enantiomers using a Chiral MD (2) column as a chiral stationary phase (CSP) by normal phase HPLC method was achieved, and the method was applied to the quality control of two commercial pharmaceuticals containing ofloxacin racemate and S-enantiomer, respectively. The results showed that the addition of acid and alkaline additives to the mobile phase simultaneously was crucial for improving the enantiomeric resolution. Molecular docking research revealed that the binding energy difference between each enantiomer and CSP was maximized when the ofloxacin molecule was non-ionized, explaining the necessity of both acid and alkaline additives in the enantioseparation. Computer simulation results further demonstrated the involvement of hydrogen bonding, hydrophobic effects, and pi-pi stacking in the stereoselective interaction, leading to the chiral separation of ofloxacin enantiomers.
NEW JOURNAL OF CHEMISTRY
(2022)
Article
Chemistry, Analytical
Jennyfer A. Aldana-Mejia, Gari Ccana-Ccapatinta, Victor Pena Ribeiro, Caroline Arruda, Rodrigo C. S. Veneziani, Sergio Ricardo Ambrosio, Jairo Kenupp Bastos
Summary: A reverse-phase high-performance liquid chromatography analytical method was developed for the detection and quantification of nine red propolis chemical markers in Brazilian red propolis extracts and D. ecastaphyllum. The method showed good detection response, linearity, precision, and robustness, making it reliable for quality control. Chemical markers were found in D. ecastaphyllum stems at lower concentrations, and seasonal analysis of Brazilian red propolis showed higher phenolic compound concentration during rainy periods.
JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS
(2021)
Article
Biochemical Research Methods
Petra Vankatova, Kveta Kalikova, Anna Kubickova
Summary: This study investigates the enantioseparation of fluorinated chiral liquid crystals in the polar organic solvent chromatography mode. Baseline enantioseparation was achieved using binary mobile phases without additives. The study also compares the effect of different polysaccharide-based chiral columns and mobile phases on the enantioseparation behavior. The results demonstrate the potential of using polar organic solvent chromatography for efficient enantioseparation.
JOURNAL OF CHROMATOGRAPHY A
(2023)
Article
Chemistry, Analytical
Troy T. Handlovic, M. Farooq Wahab, Daniel W. Armstrong
Summary: This paper presents a simple and rapid peak symmetrization algorithm for enantiomeric separations. It provides a method for extracting the distortion parameter and discusses techniques to reduce noise in chromatographic data. The paper also includes a survey of chiral separations and examples of symmetrization of enantiomer peaks.
ANALYTICAL CHEMISTRY
(2022)
Article
Chemistry, Analytical
Ben Chen, Haibo You, Liqun Fang, Tingting Lin, Ping Xu, Chu Chu, Shengqiang Tong
Summary: In this study, reverse phase high-performance liquid chromatography with sulfobutylether-beta-cyclodextrin as chiral mobile phase additive was used to analytically separate five N-alkyl drugs enantiomers. Various factors affecting retention and enantioselectivity were investigated. The results showed that sulfobutylether-beta-cyclodextrin can effectively enhance the separation of enantiomers.
JOURNAL OF SEPARATION SCIENCE
(2022)
Article
Multidisciplinary Sciences
M. E. K. Wahba, D. El Sherbiny, D. El Wasseef
Summary: The study introduces two new concepts related to chiral separation: successful chiral separation of enantiomeric drugs using micelle-based liquid chromatography without chiral selectors, and the compatibility of hybrid micelle liquid mobile phases with chiral columns. These concepts could potentially revolutionize chiral separation methods and offer an environmentally safe alternative to traditional elution methods.
JOURNAL OF TAIBAH UNIVERSITY FOR SCIENCE
(2021)
Article
Chemistry, Analytical
Raymond B. Yu, Joselito P. Quirino
Summary: This study demonstrates the successful chiral separation of various analytes using different cyclodextrins as mobile phase additives in open-tubular liquid chromatography with a stable coating. The method achieved high resolutions and low %RSD values.
JOURNAL OF SEPARATION SCIENCE
(2022)
Article
Pharmacology & Pharmacy
Prachi Raikar, Bannimath Gurupadayya, Subhankar P. Mandal, Maruthi Reddy, Prabitha Prabhakar
Summary: A normal phase-High Performance Liquid Chromatographic (HPLC) method was developed for the enantioseparation of Oxomemazine, showing good accuracy and linear response, validated according to ICH guidelines.
CURRENT PHARMACEUTICAL ANALYSIS
(2021)
Article
Chemistry, Analytical
Joel B. Langford, Ira S. Lurie
Summary: The use of micro, capillary, and nano liquid chromatography systems in forensic analysis shows great potential, especially in cases where sample size is limited. Reduction in flow rates can significantly lower operating costs and improve detection limits when using mass spectrometric analysis. Recent advances in miniaturized liquid chromatography systems also aim at in-laboratory and on-site detection, with promising areas not yet applied to forensic research being discussed.
JOURNAL OF SEPARATION SCIENCE
(2022)
Article
Chemistry, Applied
Shan Li, Zhe Liu, Ying Ye, Lixia Luo, Lijuan Han
Summary: In this study, a cholesteric chiral molecular tweezer 7a was synthesized and its fluorescence spectra were investigated in the presence of various amino acids. The molecular tweezer 7a exhibited specific recognition ability for tryptophan in the buffer solution, with a low detection limit. A new method for rapid determination of tryptophan in food samples was established by eliminating interference from metal cations and anions. The method showed high accuracy and reliability with good recoveries and low relative standard deviations. Additionally, the chiral resolution of D-/L-tryptophan enantiomers was achieved using molecular tweezer 7a as a chiral selector in high performance liquid chromatography.
JOURNAL OF FOOD COMPOSITION AND ANALYSIS
(2023)
Article
Chemistry, Analytical
Sandra Salido-Fortuna, Maria Luisa Marina, Maria Castro-Puyana
Summary: This study developed a chiral selective method using Electrokinetic Chromatography for the simultaneous separation of licarbazepine acetate and licarbazepine. The method effectively separated the four enantiomers in a short time and showed suitability for various applications.
Review
Pharmacology & Pharmacy
Chiara Fanali, Giovanni D'Orazio, Alessandra Gentili, Salvatore Fanali
Summary: This review paper discusses the application of miniaturized techniques, including capillary electrophoresis and nano-liquid chromatography, in the separation and analysis of NSAIDs, highlighting their high mass sensitivity and potential for coupling with Mass Spectrometry.
CURRENT PHARMACEUTICAL ANALYSIS
(2021)
Article
Biochemical Research Methods
Alvaro Santana-Mayor, Ruth Rodriguez-Ramos, Barbara Socas-Rodriguez, Miguel Angel Rodriguez-Delgado, Giovanni D'Orazio
Article
Biochemical Research Methods
Giovanni D'Orazio, Chiara Fanali, Salvatore Fanali, Alessandra Gentili, Marina Karchkhadze, Bezhan Chankvetadze
JOURNAL OF CHROMATOGRAPHY A
(2020)
Article
Biochemical Research Methods
Pierpaolo Tomai, Alessandra Gentili, Salvatore Fanali, Yolanda Pico
JOURNAL OF CHROMATOGRAPHY A
(2020)
Article
Biochemical Research Methods
Salvatore Fanali, Bezhan Chankvetadze
Summary: Capillary electrochromatography (CEC) has gone through a dramatic development from promise to growth to stagnation and decline. Various reasons such as competitive trends, inadequate development, and lack of innovative activities have led to the stagnation of CEC in the field.
JOURNAL OF CHROMATOGRAPHY A
(2021)
Review
Biochemical Research Methods
Chiara Fanali, Giovanni D'Orazio, Alessandra Gentili, Salvatore Fanali
Summary: Capillary electromigration and liquid chromatographic techniques are miniaturized methods that offer advantages in separation science with high efficiency and resolution. They have been widely used for the analysis of various compounds and show potential for drug abuse analysis.
Article
Biochemistry & Molecular Biology
Valeria Gallo, Pierpaolo Tomai, Valerio Di Lisio, Chiara Dal Bosco, Paola D'Angelo, Chiara Fanali, Giovanni D'Orazio, Ilaria Silvestro, Yolanda Pico, Alessandra Gentili
Summary: The study successfully applied a green sample preparation technique to extract 14 illicit drugs from urine samples, achieving good results that were validated following FDA guidelines. The extraction process was optimized and met the criteria for bioanalytical methods, demonstrating good performance across various parameters.
Article
Biochemistry & Molecular Biology
Chiara Dal Bosco, Flavia Bonoli, Alessandra Gentili, Chiara Fanali, Giovanni D'Orazio
Summary: A novel chromatographic application using the nano-LC technique for chiral separation was reported in this study. Chiral recognition of 12 antifungal drugs was achieved through optimized mobile phase composition and experimental conditions. The method demonstrated efficient separation of multiple enantiomers and was successfully applied to the analysis of milk samples.
Article
Biochemical Research Methods
Massimo Giuseppe De Cesaris, Giovanni D'Orazio, Chiara Fanali, Alessandra Gentili, Nino Takaishvili, Bezhan Chankvetadze, Salvatore Fanali
Summary: In this study, enantiomers of chiral agrochemicals were successfully separated using nano-liquid chromatography and capillary electrochromatography. The use of a capillary column packed with immobilized amylose tris(3-chloro-5-methylphenylcarbamate) as the chiral selector showed better performance in CEC than in nano-LC. The findings suggest the potential of CEC for enantioseparations in the analysis of chiral agrochemicals.
JOURNAL OF CHROMATOGRAPHY A
(2022)
Article
Chemistry, Physical
L. Bouaziz, M. Dubus, K. Si-Ahmed, H. Kerdjoudj, M. Ozacar, Y. Bessekhouad
Summary: IxZnO materials were prepared by microwave post-heating process, and their structural properties, antibacterial effect, and photocatalytic activity were investigated. The results showed improved transport properties and photoactivity, as well as enhanced bactericidal activity.
JOURNAL OF MOLECULAR STRUCTURE
(2022)
Article
Materials Science, Multidisciplinary
L. Bouaziz, S. Boulahlib, M. Ozacar, K. Si-Ahmed, Y. Bessekhouad
Summary: This study focuses on the impact of iodine doping on the properties of ZnO, including structural, optoelectronic, optical, dielectric and transport properties. I-doped ZnO materials were synthesized using a sol gel method and further analyzed using various techniques. The materials were successfully used for fingerprint detection and showed potential for forensic applications.
MATERIALS TODAY COMMUNICATIONS
(2022)
Article
Biochemical Research Methods
Elena Lucci, Chiara Dal Bosco, Lorenzo Antonelli, Chiara Fanali, Salvatore Fanali, Alessandra Gentili, Bezhan Chankvetadze
Summary: Up to 40% of plant protection products currently used contain chiral active ingredients, which may exhibit different activity, toxicity, and biotic degradation rates due to their interaction with enzymes or other naturally occurring asymmetric molecules. High-performance liquid chromatography (HPLC) is commonly employed for enantioseparations of chiral pesticides, with derivatized amylose/cellulose-based columns being the most widely used due to their universal analyte coverage. Trace analysis using sensitive detection techniques such as mass spectrometry has revealed the ubiquitous occurrence of chiral pesticides in various environmental matrices. The research in this field has grown significantly in recent years, driven by the need to assess and mitigate the risks associated with exposure to these emerging contaminants.
JOURNAL OF CHROMATOGRAPHY A
(2022)
Review
Chemistry, Analytical
Susanna Della Posta, Chiara Fanali, Valeria Gallo, Salvatore Fanali
Summary: This paper presents recent results obtained by coupling electromigration techniques with mass spectrometry, highlighting the advantages of this hybrid approach and discussing selected applications.
TRAC-TRENDS IN ANALYTICAL CHEMISTRY
(2022)
Article
Biochemical Research Methods
Sandra Salido-Fortuna, Chiara Dal Bosco, Alessandra Gentili, Maria Castro-Puyana, Maria Luisa Marina, Giovanni D'Orazio, Salvatore Fanali
Summary: In this study, the enantioseparation of 10 drugs from different families was carried out using nano-LC and a column with immobilized amylose tris(3-chloro-5-methylphenylcarbamate) silica. The effect of adding different salts to the mobile phase was evaluated for chiral separation. Buffer concentration in the mobile phase and liquid-liquid microextraction using isoamyl acetate were studied to improve the separation and increase sensitivity, achieving satisfactory recoveries (>70%) for four chiral drugs from tap and environmental waters.
Correction
Biochemical Research Methods
Yong Wang, Suhua Yu, Rui Li, Jing Wan, Yuheng Wang, Zongli Huo, Chunyong Wu, Li Mi, Songqin Liu
JOURNAL OF CHROMATOGRAPHY A
(2024)
Review
Biochemical Research Methods
Israel D. Souza, Maria Eugenia C. Queiroz
Summary: Organic-silica hybrid monolithic materials have gained significant attention in separation science and sample preparation due to their unique properties. This review summarizes the characteristics, current status, and recent developments of these materials, as well as discusses synthesis methods, characterization techniques, and strategies for improving extraction efficiency in various applications.
JOURNAL OF CHROMATOGRAPHY A
(2024)
Article
Biochemical Research Methods
Bhagwat Upreti, Bhanu Prasad Vempatapu, Jagdish Kumar, Pankaj K. Kanaujia
Summary: Lubricating oils are essential for the effective performance of internal combustion engines. This study presents a new HPLC method for determining additives in finished lubricating oils and polar substances in used engine oils.
JOURNAL OF CHROMATOGRAPHY A
(2024)
Article
Biochemical Research Methods
Zongqing Huang, Haoju Hua, Xiuzhen Du, Zipeng Zhen, Wei Zhao, Jun Feng, Ji-an Li
Summary: This study successfully isolated VHHs against the SUMO protein for the first time using biopanning of an immune camelid nanobody library. The VHHs were coupled to agarose resins to form affinity chromatography resins, allowing for one-step purification of various SUMO fusions.
JOURNAL OF CHROMATOGRAPHY A
(2024)
Article
Biochemical Research Methods
Xueting Qiu, Xuben Hou, Yue Yang, Hao Fang, Fei Cui, Xinying Yang
Summary: In this study, a new method based on electrophoretically mediated microanalysis was developed for the investigation of PTPRO enzymatic activity. The method was successfully used to determine the kinetics of PTPRO and the inhibitory concentration of PTPRO inhibitors. The method exhibited improved accuracy and reduced consumption compared to traditional methods.
JOURNAL OF CHROMATOGRAPHY A
(2024)
Article
Biochemical Research Methods
Feifei Luo, Mengmeng Hao, Lei Zhang, Yangguo Xie, Wei Hou, Hongya Wang, Zhongli Zhang
Summary: In this study, a comprehensive screening and structure elucidation of 23 nonvolatile organic compounds (NVOCs) in two antibody drugs was conducted. Seven previously unreported compounds were identified. A quantitative method with high sensitivity, accuracy, and precision was developed for evaluating the safety of NVOCs in drug products.
JOURNAL OF CHROMATOGRAPHY A
(2024)
Article
Biochemical Research Methods
Zuzana Vosahlova, Kveta Kalfkova, Martin Gilar, Jakub Szymarek, Maria Mazurkiewicz-Beldzinska, Sylwia Studzi
Summary: A hydrophilic interaction liquid chromatography method was developed for the separation and identification of oligonucleotide impurities and metabolites, and successfully applied to the analysis of serum samples from Spinraza-treated patients.
JOURNAL OF CHROMATOGRAPHY A
(2024)
Article
Biochemical Research Methods
Aswanidevi Kongasseri, Thirumalai Madhesan, Sangeetha Krishna Kumar, Sushmitha Pedugu Sivaraman, Suchashrita Mitra, Pitchaiah Kancharlapalli Chinaraga, C. V. S. Brahmmananda Rao, Sivaraman Nagarajan, Prabhakaran Deivasigamani, Akhila Maheswari Mohan
Summary: This study focuses on the sequential separation of trivalent lanthanides using modified C-18 silica-packed supports and reversed-phase HPLC technique. By tuning the column modifiers and separation parameters, the researchers achieved systematic separation of Ln(3+). The results showed that the choice of column modifiers and fine-tuning of the modification procedure were crucial for achieving excellent separation.
JOURNAL OF CHROMATOGRAPHY A
(2024)
Article
Biochemical Research Methods
Raquel Perez-Robles, Szabolcs Fekete, Robert Kormany, Natalia Navas, Davy Guillarme
Summary: There is a mismatch between the sample diluent and the mobile phase in HILIC analysis, leading to analyte breakthrough and peak distortion. Adding a weak solvent for pre-injection can effectively prevent these issues and improve sensitivity.
JOURNAL OF CHROMATOGRAPHY A
(2024)
Article
Biochemical Research Methods
Oleg Pokrovskiy, Irina Rostovschikova, Konstantin Ustinovich, Ilya Voronov, Dmitry Kosyakov
Summary: A chromatography-like propagation of water through the material bed was observed during supercritical fluid extraction of aroma plants with high moisture content, which could be significant for modeling the kinetics of supercritical fluid extraction of non-volatile compounds.
JOURNAL OF CHROMATOGRAPHY A
(2024)
Article
Biochemical Research Methods
Yasar Kemal Recepoglu, Ozguer Arar, Asli Yuksel
Summary: Biosorption using phosphorylated hazelnut shell waste (FHS) is a promising method for lithium removal and recovery. This study investigated the performance of a continuous-flow packed-bed column system using FHS for ultra-low level lithium removal. The results showed that the lihium biosorption capacity of the FHS column was unaffected by the bed height, but decreased with increasing flow rate.
JOURNAL OF CHROMATOGRAPHY A
(2024)
Article
Biochemical Research Methods
Jian Sun, Zheheng Zheng, Zixiao Jia, Jiabin Wang, Xucong Lin
Summary: In this study, an ionic covalent organic framework (iCOF) surface grafting monolithic sorbent was prepared for in-tube solid-phase microextraction (SPME) of aristolochic acids (AAs) in various samples. The density of quaternary ammonium ions in the iCOF was modulated for enhanced adsorption of AAs. The iCOF surface grafting monolithic sorbent was confirmed by different means. Several operating conditions were optimized to develop the online in-tube SPME-HPLC method, which showed good linearity, low limits of detection, and high recoveries for AAs in serum samples. This study presents a feasible approach for the application of COF-based monolithic sorbents in sample preparation.
JOURNAL OF CHROMATOGRAPHY A
(2024)
Article
Biochemical Research Methods
Zeng Wen, Ruihan Peng, Die Gao, Jing Lin, Jia Zeng, Zhou Li, Famin Ke, Zhining Xia, Dandan Wang
Summary: A chitosan-alginate sponge with multiple cross-linking networks was developed for adsorption and enrichment of anionic dyes from food samples. The sponge showed better three-dimensional network structure, mechanical behavior, and stability compared to pure chitosan and alginate sponges. The adsorption performance and selectivity of the sponge were systematically studied, and it maintained high adsorption capacity and selectivity for anionic dyes. The sponge also showed satisfactory reusability and was successfully combined with high-performance liquid chromatography for the enrichment and detection of anionic dyes in candy and cocktail samples.
JOURNAL OF CHROMATOGRAPHY A
(2024)
Article
Biochemical Research Methods
Hairong Zhang, Xiaojuan Jiang, Dandan Zhang, Yuexin Yang, Qiang Xie, Caisheng Wu
Summary: Analysis of in vivo exposure to traditional Chinese medicine using mass spectrometry is helpful for identifying effective ingredients and developing new drugs. This study focused on Forsythia suspensa (Lian Qiao) and used metabolomics technology to explore its in vivo exposure. By comparing the differences before and after administration, a complete set of nontargeted analysis strategies for TCM exposure was established. The study identified 393 Lian Qiao-related chemical components in mice after administration, including prototypes and metabolites. This study provides a reference for research on the active ingredients of Lian Qiao in vivo.
JOURNAL OF CHROMATOGRAPHY A
(2024)
Article
Biochemical Research Methods
Oscar Castejon-Musulen, Ricardo Lopez, Ignacio Ontan, Vicente Ferreira
Summary: A quantitative analytical method was developed and validated in this study to determine the concentrations of 81 aroma-relevant wine volatiles. The method utilizes stir bar sorptive extraction and multidimensional gas chromatography with flame ionization detector or mass spectrometer. The method demonstrated good linearity, reproducibility, and recovery, and was successfully applied to analyze 20 wine samples.
JOURNAL OF CHROMATOGRAPHY A
(2024)