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hplc-MS/MS method for simultaneous analysis of plasma 2-hydroxybuty-rate and 2-hydroxyisobutyrate: Development and clinical significance

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CLINICA CHIMICA ACTA 2025年 565卷 120023页

作者： Campi, Beatrice Vitelli, Valentina Saponaro, Federica Zucchi, Riccardo Ferrannini, Ele Saba, Alessandro CNR Inst Clin Physiol Via Giuseppe Moruzzi 1 I-56124 Pisa Italy Univ Pisa Dept Surg Med & Mol Pathol & Crit Care Med Via Savi 10 I-56126 Pisa Italy Univ Pisa Ctr Instrument Sharing Lungarno Pacinotti 43-44 I-56126 Pisa Italy

Recent studies have identified relationships between diabetes mellitus and short-chain fatty acids, including 2hydroxybutyrate (2-HB) and 2-hydroxyisobutyrate (2-HiB);2-HB has been associated to the early stages of insulin resistance, while 2-HiB with the risk and progression of complications of Type 1 diabetes. Their metabolism and pathophysiological role in humans are not fully clarified. The possible association between 2-HB and 2-HiB and diabetes mellitus was investigated with a novel mass spectrometry-based assay, capable of discriminating plasma 2-HiB and 2-HB from their HB isomers. Accuracy and precision (RSD%) were always in the range 99-102% and 0.7-3.5%, respectively. The study involved samples from subjects with normal glucose tolerance (NGT) and Type 2 diabetes (T2D), originally included in a multicenter study investigating mechanisms involved in atherothrombosis. NGT subjects exhibited concentrations of 2-HB and 2-HiB of 61 (36) and 3.1 (1.9) mu mol/L, median (interquartile range), respectively, that were significantly lower than those of the T2D patients, whose values were 74 (4.0) and 3.8 (2.9) mu mol/L, respectively. The pattern of association of these molecules with clinical and metabolic variables is partially different: both compounds were directly related to male sex, BMI, HbA1c, and plasma glucose, 2-HiB also with age, systolic blood pressure, and HDL-cholesterol. Furthermore, they correlate with free fatty acids, glycerol, and triglyceride concentrations, but the latter correlation was negative for 2-HB and positive for 2-HiB. Results confirmed the clinical significance of 2-HB and 2-HiB, in differential association with metabolic features of T2D.

关键词： 2-hydroxybutyrate 2-hydroxyisobutyrate hplc Mass spectrometry

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A validated rp-hplc method for simultaneous determination of olopatadine hydrochloride and its related substances in eye drop

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JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES 2025年第1-5期48卷 28-36页

作者： Hasan, Md. Abid Helal, Naima Azmi, Sajia Nasir, Sumaya Samrina Sultana, Nursad Jahan Univ Asia Pacific Dept Pharm Dhaka Bangladesh World Univ Bangladesh Dept Pharm Dhaka Bangladesh Univ Sci & Technol Chittagong Dept Pharm Chattogram Bangladesh

Olopatadine Hydrochloride, a H1-receptor antagonist, widely used for Allergic Conjunctivitis. A hplc method was created and validated for the quantification of olopatadine hydrochloride and its related substances in eye formulation in accordance with ICH standards. The separation of olopatadine hydrochloride was done by using a 4.6-mm 15-cm;5 mu m packing USP L7 column with a mobile phase made up of a mixer of phosphate buffer, pH 3.0: Acetonitrile (72:28) ratio at a flow rate of 1.0 mL/min and injection volume 30 mu L. A photodiode array detector was used at a wavelength of 299 nm. The validation parameters including specificity, LOD/LOQ, linearity, accuracy, precision, robustness, and solution stability, were verified for performance of the method. The linearity ranges were 0.02-0.40, 0.0004-0.008 and 0.0001-0.002 mg/mL for olopatadine hydrochloride, olopatadine-related compound B and olopatadine carbaldehyde, respectively. The % recovery was within the 80-120%. When the column temperature and flow rate were changed, the system suitability resolution was still within the acceptable range. The solutions were stable after 24 hr at both room temperature and 5 degrees C temperature. For the analysis of olopatadine hydrochloride and its impurity in pharmaceutical finished eye dosage form, the confirmed hplc method can be a workable analytical approach.

关键词： Chromatography eye drop hplc olopatadine hydrochloride validation

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Solid phase extraction of Aflatoxin M1 in milk samples by graphene oxide-poly-L-lysine nanocomposite followed by hplc

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INTERNATIONAL JOURNAL OF ENVIRONMENTAL ANALYTICAL CHEMISTRY 2025年第2期105卷 418-431页

作者： Al-Gburi, Hanan Naser Hussein Eftekhari, Mohammad Gheibi, Mohammad Univ Babylon Fac Sci Dept Chem Hillah Iraq Univ Neyshabur Fac Sci Dept Chem Neyshabur Iran Reyhan Azma Iranian Lab Mashhad Iran Tech Univ Liberec Inst Nanomat Adv Technol & Innovat Liberec Czech Republic

An efficient, novel and green Graphene Oxide-Poly-L-Lysine (GO-PLL) adsorbent was successfully synthesised and used for solid-phase extraction of aflatoxin M1 (AFM1) in liquid milk samples followed by high performance liquid chromatography (hplc) equipped with fluorescence detector (FLD). The synthesised adsorbent was characterised by Fourier Transform Infrared Spectrophotometry (FT-IR), Field Emission Scanning Electron Microscopy (FESEM), Energy-dispersive X-ray spectroscopy (EDX) and X-Ray diffraction (XRD) analysis. Different parameters affecting the recovery percentage of AFM1 including pH of sample solution, amounts of adsorbent, contact time and desorbent solution (types and volume) were completely investigated and optimised. It was found that, with an enrichment factor of 15.2, the calibration curve is linear in the range of 0.05-4.00 ng ml-1 AFM1 and the limit of detection (LOD) and limit of quantification (LOQ) values were 0.019 and 0.063 ng mL-1, respectively. The relative standard deviations (RSDs) ranged from 4.5% to 5.7% and 4.2% to 6.7% for intra-day and inter-day variations, respectively. Finally, the proposed solid-phase extraction method was successfully applied for determination of trace levels of AFM1 in different milk samples.

关键词： Aflatoxin M1 Graphene Oxide-Poly-L-Lysine (GO-PLL) adsorbent hplc milk sample

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Effects of Porous Structure of Separation Column on Chromatograms Obtained by Phase-Separation Mode in hplc

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CHROMATOGRAPHIA 2025年第3期88卷 215-224页

作者： Katayama, Tetsuro Iharada, Takeshi Obata, Yuki Sakamaki, Hiroshi Tsukagoshi, Kazuhiko Doshisha Univ Grad Sch Sci & Engn Appl Chem Kyotanabe 6100321 Japan Chem Evaluat & Res Inst 1600 ShimotakanoSugito Machi Saitama 3450043 Japan

A novel hplc system utilizing a phase-separation multiphase flow as the eluent has been developed, referred to as phase-separation mode. This research explores the influence of the porous structure in an octadecyl-modified silica (ODS) column (with a pore diameter of 12 nm) on chromatographic outcomes under the phase-separation mode in hplc. The chromatograms obtained from the porous ODS column were compared to those generated with a non-porous ODS column. In preliminary experiments, twenty-four mixed solutions, comprising combinations of water/acetonitrile/ethyl acetate and water/acetonitrile, were introduced as eluents at a column temperature of 20 degrees C. A model mixture of 2,6-naphthalenedisulfonic acid (2,6-NDS) and 1-naphthol (1-NA) was injected into the system, with separation achieved in most solutions except for some highly organic solvent-rich solutions where 2,6-NDS eluted faster than 1-NA, indicating reverse-phase mode operation. Subsequently, the separation of the model mixture was assessed at 0 degrees C, and four specific ternary mixtures were analyzed in detail at both 20 degrees C and 0 degrees C. These ternary mixtures, defined by their volume ratios, exhibited a two-phase separation, establishing a phase-separation multiphase flow. Consequently, the solution flow was homogeneous at 20 degrees C and heterogeneous at 0 degrees C. For instance, solutions with water/acetonitrile/ethyl acetate ratios of 20:60:20 (organic solvent-rich) and 70:23:7 (water-rich) were introduced as eluents at both 20 degrees C and 0 degrees C. At 0 degrees C in the organic solvent-rich eluent, 1-NA eluted faster than 2,6-NDS, characteristic of the phase-separation mode. In contrast, the water-rich eluent resulted in faster elution of 2,6-NDS at both temperatures. The porous ODS column displayed improved separation efficiency at 0 degrees C compared to the non-porous column, which can be attributed to the porous effect under phase-separation conditions.

关键词： Phase-separation multiphase flow Phase-separation mode Porous ODS column hplc

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An RP-hplc Method for the Simultaneous Analysis of Selected Antiviral Drugs

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CHROMATOGRAPHIA 2025年第3期88卷 179-191页

作者： Ozdemirhan, Mehmet Emre Ozen, Guerkan Nemutlu, Emirhan Turkish Med & Med Devices Agcy Dept Anal & Control Labs Ankara Turkiye Baskent Univ Fac Pharm Dept Analyt Chem Etimesgut Ankara Turkiye Hacettepe Univ Fac Pharm Dept Analyt Chem Ankara Turkiye

A rapid and efficient reversed-phase high-performance liquid chromatography (RP-hplc) method was developed and validated for the simultaneous determination of six antiviral drugs: emtricitabine (EMT), entecavir (ENT), favipiravir (FAV), ganciclovir (GAN), valaciclovir (VAL), and valganciclovir (VLG). Chromatographic separation was achieved on an ExsilTM Mono 100 C18 column using a mobile phase of 50 mM phosphate buffer (pH 4): acetonitrile (90:10, v/v) at a flow rate of 0.5 mL/min. UV detection was performed at 215 nm. The method was validated according to ICH Q2(R2) guidelines, demonstrating excellent linearity (R-2 > 0.9938) across the concentration ranges of 1.0-150 mu g/mL for EMT, ENT and VLG, and 5.0-200 mu g/mL for FAV, GAN and VAL. The LOD and LOQ values ranged from 0.02 to 0.48 mu g/mL and 0.05 to 1.45 mu g/mL, respectively. Intra-day and inter-day precision, expressed as relative standard deviation (RSD), were less than 1.82%, while accuracy, expressed as relative error (RE), was within +/- 1.34%. Recovery studies yielded values ranging from 98.12% to 101.60%, further confirming method accuracy. The method proved to be selective, robust, and suitable for the quantitative analysis of these antiviral drugs in pharmaceutical formulations, with results obtained for commercially available tablets demonstrating excellent agreement with labeled contents. Notably, stability studies revealed the susceptibility of EMT, ENT, and FAV to degradation under refrigerated storage, highlighting the need for timely analysis of these compounds. In addition, the greenness, blueness, and whiteness of the method were evaluated, and the developed method performs strongly across environmental (AGREE score: 0.79), practical (BAGI index: 85), and sustainability (whiteness value: 74.7) criteria, reinforcing its viability as a sustainable approach for antiviral analysis. This validated RP-hplc method provides a reliable and efficient tool for the quality control of these essential ant

关键词： Antivirals hplc Validation Pharmaceuticals

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A Low-cost and Rapid Method for Determination of Five Flavonoids in Herbal Medicines with Rutin by hplc-UV at Equal Absorption Wavelength

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CURRENT ANALYTICAL CHEMISTRY 2025年第2期21卷 124-133页

作者： Qian, Zhengming He, Zhuobin Lian, Dongyin Huang, Qi Tan, Guoying Xie, Juying Xiangnan Univ Coll Med Imaging Lab & Rehabil Chenzhou Peoples R China Dongguan HEC Cordyceps R&D Co Ltd Key Lab State Adm Tradit Chinese Med Dongguan Peoples R China

Background Flavonoid is a type of active constituent in herbs and always used as the quality control markers of herbal medicines. Owing to the extensive diversity of flavonoids, numerous reference compounds are necessitated for the analysis of flavonoids, and some are usually very expensive, which engenders challenges in the analysis of flavonoids in herbal medicines. Consequently, the development of a simple, rapid, and reference compounds saving method is important for the determination of flavonoids in herbal *** In order to develop a high-performance liquid chromatography (hplc) method for the determination of 5 flavonoids (mangiferin, hesperidin, baicalin, buddleoside, and rutin) in five herbal medicines (Anemarrhenae rhizome, Sophorae flos, Citri reticulatae pericarpium, Scutellariae radix, and Chrysanthemi indici flos) with *** Five herbal medicine samples were prepared according to the Chinese Pharmacopoeia which includes ultrasound and reflux methods. The separation of the sample was performed on a PoroShell 120 EC-C18 (4.6 mmx100 mm, 2.7 mu m) by gradient elution with 0.1% formic acid and acetonitrile at a flow rate of 1.0 mL/min. The wavelengths were set as follows: Anemarrhenae rhizome (363 nm), Sophorae flos (256 nm), Citri reticulatae pericarpium (236 nm), Scutellariae radix (263 nm), Chrysanthemi indici flos (354 nm).Results The method validation showed that the established hplc method was accurate and stable for quantitative analysis of flavonoids in five herbal medicines. The comparative analysis revealed that the determination results of the current hplc method and Chinese Pharmacopoeia method are consistent, exhibiting less than 1% relative error. Remarkably, the developed hplc method needs one cheapest reference compound (rutin) and costs 8 min for sample hplc *** The developed hplc method for quantitative analysis of five flavonoids in five herbal medicines is simple, rapid, and reference compound saving

关键词： Flavonoids rutin herbal medicine hplc equal absorption wavelength quantitative analysis quality control

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Identification and characterization of unknown oxidation degradation products of Rimegepant by hplc and triple quadrupole mass spectrometry

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EUROPEAN JOURNAL OF MASS SPECTROMETRY 2025年第1-2期31卷 38-50页

作者： Godi, Narayana Reddy Dodda, Sireesha Vanga, Nagavardhana Reddy Ummiti, Kumarswamy Anurag Univ Sch Pharm Dept Pharmaceut Anal Hyderabad 500088 Telangana India GITAM Deemed Be Univ Ind Chem Prod Dev & Anal Ctr GITAM Sch Sci Dept Chem Bengaluru Campus Bengaluru Karnataka India Koneru Lakshmaiah Educ Fdn Coll Engn Dept Chem Guntur Andhra Pradesh India

Rimegepant is a calcitonin gene-related peptide receptor antagonist that has been licensed for migraine headache treatment in the United States, the European Union, the United Kingdom, Hong Kong, Australia, and Kuwait. The oxidation stress study of the Rimegepant drug substance revealed the presence of five impurities. Rimegepant degraded by 5% under the selected oxidation conditions, meeting regulatory expectations. Four out of five impurities are enhanced by more than 1%. This research aims to characterize these oxidation degradation products utilizing the triple quadrupole mass spectroscopic technique. The Rimegepant oxidation degradation products were identified using an optimized chromatographic method that relies on reverse-phase hplc with PDA detection. This technique utilized a Waters Xbridge C18 column with an eluent mixture of acetonitrile and 0.1% formic acid in water. The oxidation products of Rimegepant have been effectively separated, with a resolution above 3.0. Triple quadrupole mass spectrometry analysis characterized the five degradation products, which showed three N-oxide impurities with masses m/z 566, m/z 550, and m/z 548, as well as two hydrolysis products with masses, m/z 218, m/z 290. These new impurities deserve special attention because the drug's potency and related impurity levels determine any pharmaceutical medication product's quality, safety, and effectiveness.

关键词： Rimegepant oxidation stress study degradation products hplc TQ-MS

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Investigation of motilin's surface adsorption on glass and polypropylene surfaces using a simple and specific hplc method

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JOURNAL OF LIQUID CHROMATOGRAPHY & RELATED TECHNOLOGIES 2025年

作者： Karaca, Sakine Atila Ugur, Duygu Yeniceli Anadolu Univ Fac Pharm Dept Analyt Chem Eskisehir Turkiye

The nonspecific binding of peptides to material surfaces is a well-known phenomenon that makes measurement of these substances challenging. Peptide adsorption can be reduced with suitable materials or additives, but the complex nature of biomolecules makes it challenging to find an universal sample preparation method. This study focused on investigating the surface adsorption behavior of motilin to enhance the sensitivity and precision of analytical methods. A simple and specific hplc method was developed for the quantification of motilin. Using this chromatographic method, it was discovered that motilin binds to both polypropylene and glass surfaces at high levels, with recovery rates of 32 and 24%, respectively. To mitigate this, the effect of protein (bovine serum albumin), salt (sodium chloride), and surfactant (Tween 80) on surface adsorption was investigated. Although all additives reduced adsorption, only Tween 80 achieved nearly 100% recovery with consistent results (RSD <= 2%). Consequently, the sample preparation procedure developed using Tween 80 was integrated into the hplc method, and the method was validated according to the International Conference on Harmonization guideline [ICH Q2(R1)]. This method is expected to have potential applications in analytical chemistry, drug development, biotechnology, and the pharmaceutical industry for providing accurate and dependable peptide measurements.

关键词： Motilin surface adsorption binding hplc peptide analysis

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Chiral Resolution of Transition Metal Polypyridyl Complexes via hplc As a Gateway to Enantiopure DNA Targeting Probes

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EUROPEAN JOURNAL OF INORGANIC CHEMISTRY 2025年第11期28卷

作者： Smith, Simon N. Graczyk, Daniel Stitch, Mark Auville, Amelia Stadler, Victoria Quinn, Susan J. Univ Coll Dublin UCD Sch Chem Dublin D04 V1 W8 Ireland

The intrinsic structural and photophysical properties of octahedral tris-(bidentate) transition metal polypyridyl complexes make them attractive DNA probes whose binding affinity and specificity for DNA can be greatly influenced by the Delta- and Lambda-enantiomer forms. Strategies for chiral resolution include chiral precursors, fractional crystallisation with chiral salts as well as chromatographic methods. The present work details the optimisation of a chiral resolution process to facilitate the isolation of metal complex enantiomers via chiral stationary phase hplc using a semi-preparative column. The scope of the study includes both Ru(II) and Os(II) polypyridyl enantiomers containing commonly encountered coordination environments as well as a range of more exotic ligand scaffolds that illustrate the generality of the method. Notably, this work also describes the ability to separate enantiomers of a mixture of two complexes prepared as a result of 'ligand-scrambling' during synthesis.

关键词： transition metal polypyridyl complex chirality chromatography hplc

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Development of a green and rapid ethanol-based hplc assay for aspirin tablets and feasibility evaluation of domestically produced bioethanol in Thailand as a sustainable mobile phase

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GREEN PROCESSING AND SYNTHESIS 2025年第1期14卷

作者： Thanayutsiri, Thana Mantadilok, Siwa Sapsin, Jiradet Tungwattanaviboon, Thada Wongwatanasin, Jetsada Opanasopit, Praneet Ngawhirunpat, Tanasait Rojanarata, Theerasak Silpakorn Univ Fac Pharm Sanam Chandra Palace Campus Nakhon Pathom 73000 Thailand Silpakorn Univ Fac Pharm Pharmaceut Dev Green Innovat Grp PDGIG Nakhon Pathom 73000 Thailand Thai Ethanol Mfg Assoc Bangkok 10400 Thailand

Despite the growing trend of using ethanol as a greener alternative to hazardous solvents like methanol and acetonitrile in high-performance liquid chromatography (hplc) analysis, no ethanol-based assay has been developed for aspirin tablets, nor has the potential of domestically produced bioethanol as a mobile phase been explored - until now. This study introduces a novel ethanol-based hplc assay for aspirin and assesses the feasibility of using locally produced bioethanol. The optimized method, featuring a 40% (v/v) ethanol-water mobile phase adjusted to pH 3.6 with glacial acetic acid, with a 15-cm C18 column at 40 degrees C and UV detection at 237 nm, successfully separated aspirin and its degradation product, salicylic acid, in 5 min. It demonstrated excellent linearity (0.1-0.6 mgmL(-1), r(2) = 0.9997), sensitivity (LOD = 0.01 mgmL(-1), LOQ = 0.03 mgmL(-1)), accuracy, and precision, with no interference from excipients. The method's performance on commercial aspirin tablets aligned with official pharmacopoeial methods. In a case study using fuel-grade bioethanol (>99.5% purity) derived from sugarcane molasses or cassava from local manufacturers in Thailand, chromatographic and analytical results matched those obtained with imported ethanol, validating its effectiveness. This innovative approach not only reduces costs and dependence on imported solvents but also supports local bio-circular-green economies and promotes greener, more sustainable analytical practices.

关键词： ethanol hplc aspirin domestic sustainability

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