Chromatographia最新文献

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Polyolefin Characterization by High Temperature Solvent Gradient Interaction Chromatography: Transitioning Away from Chlorinated Desorption Promoting Solvents 高温溶剂梯度相互作用色谱法表征聚烯烃:从氯化解吸促进溶剂过渡
IF 1.6 4区 化学
Chromatographia Pub Date : 2026-08-24 DOI: 10.1007/s10337-026-04507-x
Subrajeet Deshmukh, Jan-Hendrik Arndt, Tibor Macko, Masud Monwar, Jeff Fodor, Robert Brüll
{"title":"Polyolefin Characterization by High Temperature Solvent Gradient Interaction Chromatography: Transitioning Away from Chlorinated Desorption Promoting Solvents","authors":"Subrajeet Deshmukh,&nbsp;Jan-Hendrik Arndt,&nbsp;Tibor Macko,&nbsp;Masud Monwar,&nbsp;Jeff Fodor,&nbsp;Robert Brüll","doi":"10.1007/s10337-026-04507-x","DOIUrl":"10.1007/s10337-026-04507-x","url":null,"abstract":"<div><p>High temperature solvent gradient interaction chromatography (HT-SGIC) has been established as a cornerstone technique to elucidate the chemical composition (CC) and underlying chemical composition distribution (CCD). In HT-SGIC, the adsorption (adsorlis) and desorption (desorlis) promoting solvents play an integral role in identifying these molecular characteristics. However, until now only a few select chlorinated solvents have been used as desorlis for polyolefin separation in spite of their health and safety considerations. Towards the goal of identifying non-chlorinated desorlis, a recent approach integrating Structure Retention Relationship (SRR) with Relative Energy Density (RED) for identifying new desorlis was employed. The effectiveness of the SRR-RED plot as a tool for classifying solvents into adsorlis and desorlis in HT-SGIC of polyolefins was investigated. Non-chlorinated desorlis identified through this method were assessed using polyethylene samples of different molar mass (MM) followed by testing on polypropylene of different tacticity. Furthermore, ethylene propylene (EP) copolymers covering a wide range of CC were employed. At the same time, correlations between the retention factor of the desorli (from SRR study) and parameters such as MM, comonomer content and elution volume were studied to examine the desorption strength of the desorlis. The non-chlorinated desorlis were further used to separate linear low-density polyethylene and ethylene propylene diene copolymers to evaluate their potential across a broad range of polyolefins. Overall, non-chlorinated desorlis 1,2,4-TMB and tetralin were realized as alternative candidates to replace chlorinated solvents for polyethylene with moderate molar mass and EP copolymers higher comonomer content. Two strategies to increase the effective retention factor of the non-chlorinated desorlis by adding a strong-retention component were assessed based on their measured retention factors but their effect on the desorption behavior of polyolefins remains to be validated.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 6","pages":"687 - 698"},"PeriodicalIF":1.6,"publicationDate":"2026-08-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10337-026-04507-x.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148974829","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Determination of Bisphenol A in Water Samples by HPLC–UV After Magnetic Solid-Phase Extraction Using Nanoparticles Derived from Iron Mining Tailings 铁尾矿纳米颗粒磁固相萃取- HPLC-UV法测定水样中的双酚A
IF 1.6 4区 化学
Chromatographia Pub Date : 2026-08-06 DOI: 10.1007/s10337-026-04504-0
Fernanda A. Luna, Luan F. Costa, Raphael R. Bretz, Camilla F. Silva, Juliana A. Torres, Francisco G. E. Nogueira, Keyller B. Borges, Maria C. Silva
{"title":"Determination of Bisphenol A in Water Samples by HPLC–UV After Magnetic Solid-Phase Extraction Using Nanoparticles Derived from Iron Mining Tailings","authors":"Fernanda A. Luna,&nbsp;Luan F. Costa,&nbsp;Raphael R. Bretz,&nbsp;Camilla F. Silva,&nbsp;Juliana A. Torres,&nbsp;Francisco G. E. Nogueira,&nbsp;Keyller B. Borges,&nbsp;Maria C. Silva","doi":"10.1007/s10337-026-04504-0","DOIUrl":"10.1007/s10337-026-04504-0","url":null,"abstract":"<div><p>A magnetic nanosorbent was synthesized from a ferric precursor recovered from iron mining tailings and applied in magnetic solid-phase extraction (MSPE) for the determination of bisphenol A (BPA) in aqueous matrices. An analytical method based on high-performance liquid chromatography with UV detection (HPLC–UV) was developed for the extraction and determination of BPA in water samples. BPA is classified as an emerging contaminant and an endocrine-disrupting compound due to its potential to interfere with the endocrine system. The Fe<sub>3</sub>O<sub>4</sub>@SiO<sub>2</sub>–NH<sub>2</sub> nanosorbent was prepared using ferric ions obtained via acid leaching of mining tailings, an abundant industrial waste. The material was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TG), scanning electron microscopy (SEM), transmission electron microscopy (TEM), pH at the point of zero charge (pHPZC), and wettability measurements. The MSPE procedure was optimized by evaluating the elution solvent, sample pH, eluent volume, sample volume, sorbent amount, and stirring time. The method exhibited good linearity (R<sup>2</sup> &gt; 0.99), with limits of detection and quantification of 30 and 80 ng mL<sup>−1</sup>, respectively. Intra- and interday precision and accuracy showed relative standard deviation (RSD) and relative error (RE) values below 15%. The proposed method was successfully applied to real water samples, and its greenness was evaluated using AGREEprep and AGREE metrics. The use of iron mining tailings as a secondary source of ferric precursor represents a sustainable and cost-effective strategy for the preparation of functional magnetic nanomaterials.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 6","pages":"661 - 675"},"PeriodicalIF":1.6,"publicationDate":"2026-08-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10337-026-04504-0.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148974792","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
LC–ESI–MS Based Degradation Profiling of Imeglimin Supported by a Validated Green Stability-Indicating RP-HPLC Method 基于LC-ESI-MS的依米霉素降解分析——绿色稳定性指示RP-HPLC法支持
IF 1.6 4区 化学
Chromatographia Pub Date : 2026-08-04 DOI: 10.1007/s10337-026-04508-w
Kiran R. Rathod, Chintankumar J. Tank
{"title":"LC–ESI–MS Based Degradation Profiling of Imeglimin Supported by a Validated Green Stability-Indicating RP-HPLC Method","authors":"Kiran R. Rathod,&nbsp;Chintankumar J. Tank","doi":"10.1007/s10337-026-04508-w","DOIUrl":"10.1007/s10337-026-04508-w","url":null,"abstract":"<div><p>Imeglimin (IMG) is the first agent of the new tetrahydrotriazine-based class of oral antidiabetic drugs known as ‘glimins’. This work presents LC–ESI–MS based degradation profiling, by fragmentation-assisted structural elucidation of major degradation products of Imeglimin under forced degradation conditions. For that, first we have developed and validated a green, robust, simple and efficient RP-HPLC method to ensure its stability. The column used in the method is ACE CN 25 column (250 mm × 4.6 mm, 5 µm). Acetonitrile: 20 mM Ammonium Formate (60:40% v/v) is used as the mobile phase at a flow rate of 1.0 ml/min. Detection was done at a detection wavelength of 245 nm. Linearity was found over the range of 5–200 µg/ml with correlation coefficient 0.9998. Specificity, linearity, precision, accuracy and robustness of the method were confirmed by rigorous validation in accordance with ICH requirements. Then, forced degradation studies were performed. Forced degradation led to the formation of five degradation products (DPs); Two in acidic, one in basic and two in oxidative conditions. IMG showed relatively higher stability under photolytic and thermal conditions. RP-HPLC combined with electrospray ionization tandem mass spectrometry (LC–ESI–MS) was used effectively to identify these degradation products, offering insights into their structural pathways. Greenness and sustainability of the method were proved with an AGREE score of 0.66 and a ComplexMoGAPI score of 65. This validated analytical method ensures reliable stability assessment of Imeglimin (IMG) with precise quantification and consistent monitoring of degradation in pharmaceutical dosage forms.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 6","pages":"699 - 712"},"PeriodicalIF":1.6,"publicationDate":"2026-08-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148974786","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Determination of Trace Anions in Electronic-Grade N-Methylpyrrolidone Using Two-Dimensional Ion Exclusion–Ion Exchange Chromatography Combined with a Valve-Switching Technique 二维离子排斥-离子交换色谱结合阀开关技术测定电子级n -甲基吡啶酮中的微量阴离子
IF 1.6 4区 化学
Chromatographia Pub Date : 2026-08-03 DOI: 10.1007/s10337-026-04506-y
Zhou Zheng, Yan Lu, Tao Ye, Mijia Feng, Songli Shen, Dan Hu, Xiaojie Xu, Xin Shen
{"title":"Determination of Trace Anions in Electronic-Grade N-Methylpyrrolidone Using Two-Dimensional Ion Exclusion–Ion Exchange Chromatography Combined with a Valve-Switching Technique","authors":"Zhou Zheng,&nbsp;Yan Lu,&nbsp;Tao Ye,&nbsp;Mijia Feng,&nbsp;Songli Shen,&nbsp;Dan Hu,&nbsp;Xiaojie Xu,&nbsp;Xin Shen","doi":"10.1007/s10337-026-04506-y","DOIUrl":"10.1007/s10337-026-04506-y","url":null,"abstract":"<div><p>Accurate determination of trace anions in electronic-grade N-methylpyrrolidone (NMP) is crucial for ensuring the reliability of lithium-ion batteries and semiconductor devices. However, severe interference from the massive organic matrix prevents conventional one-dimensional ion chromatography (1D-IC) from meeting the stringent requirements of sub-microgram-per-kilogram (µg/kg) level detection. To address this challenge, an automated, online two-dimensional ion exclusion–ion exchange chromatography (2D-ICE-IC) method integrated with a valve-switching technique was developed. By introducing ion exclusion chromatography (ICE) in the first dimension, the complex NMP matrix and potential interfering components were eliminated, leveraging the distinctly different retention behaviors between the target anions and the organic background. Combined with large-volume injection and a precisely timed valve-switching program, the heart-cut target anions were captured on a concentrator column and subsequently transferred to the second-dimensional ion exchange system for high-sensitivity analysis. Under optimized conditions, five target anions (Cl⁻, Br⁻, NO₃⁻, SO₄²⁻, and PO₄³⁻) exhibited excellent linearity within the range of 0.5–20 µg/kg (<i>r</i> &gt; 0.999), with limits of detection (LODs) as low as 0.006–0.021 µg/kg. Spiked recoveries at low, medium, and high concentration levels ranged stably between 75% and 115%, with precisions (RSD, <i>n</i> = 6) below 5%. Operated within a Class 1000 cleanroom, this method effectively prevents secondary contamination and analyte loss typically associated with traditional offline sample pretreatment. Its high automation and exceptional selectivity offer a reliable and industry-applicable strategy for the purity control and quality assessment of high-purity, highly polar organic solvents.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 6","pages":"677 - 686"},"PeriodicalIF":1.6,"publicationDate":"2026-08-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148974828","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Correction: Lift Force on Spherical Particle in Nonlinear Velocity Gradient of Laminar Liquid Flow: Application to Field-Flow Fractionation 修正:层流流体非线性速度梯度中球形颗粒的升力:在场流分馏中的应用
IF 1.6 4区 化学
Chromatographia Pub Date : 2026-07-22 DOI: 10.1007/s10337-026-04505-z
Josef Janča
{"title":"Correction: Lift Force on Spherical Particle in Nonlinear Velocity Gradient of Laminar Liquid Flow: Application to Field-Flow Fractionation","authors":"Josef Janča","doi":"10.1007/s10337-026-04505-z","DOIUrl":"10.1007/s10337-026-04505-z","url":null,"abstract":"","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 5","pages":"605 - 605"},"PeriodicalIF":1.6,"publicationDate":"2026-07-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10337-026-04505-z.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148695241","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Revisiting Solvent Impurities with Log-Based Fluorescence Detection and GC–MS Log-Based荧光检测和GC-MS重访溶剂杂质
IF 1.6 4区 化学
Chromatographia Pub Date : 2026-07-13 DOI: 10.1007/s10337-026-04503-1
Maria Olds, Siddharth Jaya Sajeevan J, Alain Berthod, Daniel W. Armstrong
{"title":"Revisiting Solvent Impurities with Log-Based Fluorescence Detection and GC–MS","authors":"Maria Olds,&nbsp;Siddharth Jaya Sajeevan J,&nbsp;Alain Berthod,&nbsp;Daniel W. Armstrong","doi":"10.1007/s10337-026-04503-1","DOIUrl":"10.1007/s10337-026-04503-1","url":null,"abstract":"<div><p>Solvents are needed in all branches of chemistry, and they must be eliminated after use. Impurities present in these solvents could concentrate detrimentally during chemical and, especially, pharmaceutical processes. So it is critically important to know the purity of the solvents used. The label-claimed purity of 24 solvents, including polar protic alcohols, polar aprotic carbonate esters and acetonitrile, dipolar ethers, aromatic solvents, and apolar alkanes, was tested by liquid chromatography with fluorescence detection (HPLC-FLD), gas chromatography with flame ionization or mass spectrometry detection (GC-FID or GC–MS). For all 24 tested solvents, the label-indicated purities were confirmed. The study showed that minute amounts of fluorescent impurities could be better visualized on a logarithmic scale of the emitted light rather than on the classical linear scale. Comparing the results obtained for the same solvent by HPLC-FLD and GC-FID showed that the fluorescence detector is so sensitive that it could detect an extremely low concentration of a fluorescent compound that did not produce a signal in the FID detector. However, the FID detected several more impurities than the fluorescence detector since many do not fluoresce. GC-FID and GC–MS chromatograms of the same sample on the same column showed similarities. But the strong advantage of the MS detector is impurity identification using extended modern spectral databases.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 6","pages":"649 - 659"},"PeriodicalIF":1.6,"publicationDate":"2026-07-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://link.springer.com/content/pdf/10.1007/s10337-026-04503-1.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148974790","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Validation of an HPLC Method for the Quantification of Tafenoquine in Bovine and Equine Plasma, Red Blood Cells, and Cell Culture Media 高效液相色谱法测定牛和马血浆、红细胞和细胞培养基中他非诺喹含量的验证
IF 1.6 4区 化学
Chromatographia Pub Date : 2026-07-07 DOI: 10.1007/s10337-026-04502-2
Andrew Ursini, Madeline Duncan, Riley Golias, Julia Cutchin, Reginaldo G. Bastos, Nicolas F. Villarino, Sherry Cox
{"title":"Validation of an HPLC Method for the Quantification of Tafenoquine in Bovine and Equine Plasma, Red Blood Cells, and Cell Culture Media","authors":"Andrew Ursini,&nbsp;Madeline Duncan,&nbsp;Riley Golias,&nbsp;Julia Cutchin,&nbsp;Reginaldo G. Bastos,&nbsp;Nicolas F. Villarino,&nbsp;Sherry Cox","doi":"10.1007/s10337-026-04502-2","DOIUrl":"10.1007/s10337-026-04502-2","url":null,"abstract":"<div><p>A simple and accurate reverse phase high-performance liquid chromatography (RP-HPLC) tafenoquine method was developed and validated for use with bovine and equine plasma, and erythrocytes, <i>Babesia caballi</i> and <i>Theileria equi</i> culture media. After protein precipitation, samples were separated on an X-Bridge C<sub>18</sub> column using a mobile phase consisting of 11 mM ammonium acetate (pH 4.0) and acetonitrile (45:55, v/v). The extraction used acetonitrile, zinc sulfate, and hydrochloric acid. Fluorescent detection occurred with an excitation of 262 nm and an emission of 476 nm. The lower limit of quantification (LLOQ) was 1 ng/mL for all matrices with a sample size of 100 µL. Intra and inter-assay variability was less than 10% for all matrices and the average recovery ranged from 81% to 98%, respectively. This validated method has been used for sample evaluation in pharmacokinetic studies to evaluate tafenoquine concentrations in both equine and bovine samples as a potential candidate for controlling hemoparasites responsible for economically important diseases.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 6","pages":"639 - 647"},"PeriodicalIF":1.6,"publicationDate":"2026-07-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148974791","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Mechanistic Mapping of Matrix Effects in LC–ESI–MS/MS Multi-residue Pesticide Analysis LC-ESI-MS /MS多残留农药分析中基质效应的机制定位
IF 1.6 4区 化学
Chromatographia Pub Date : 2026-07-06 DOI: 10.1007/s10337-026-04501-3
Abderrahim Eddahby, Abdelkrim Chahine, Lahcen Hssaini
{"title":"Mechanistic Mapping of Matrix Effects in LC–ESI–MS/MS Multi-residue Pesticide Analysis","authors":"Abderrahim Eddahby,&nbsp;Abdelkrim Chahine,&nbsp;Lahcen Hssaini","doi":"10.1007/s10337-026-04501-3","DOIUrl":"10.1007/s10337-026-04501-3","url":null,"abstract":"<div><p>Electrospray ionisation matrix effects (ME) remain a central challenge in multi-residue pesticide analysis by ultra-performance liquid chromatography tandem mass spectrometry (UPLC–ESI–MS/MS). This study presents a data-driven characterisation of ME across 90 pesticide analytes in ten structurally diverse food matrices using a QuEChERS protocol. Of 900 analyte–matrix measurements, 80.8% showed negligible ME (± 10%), 11.1% moderate (± 10–20%), 7.7% strong enhancement (&gt; + 20%), and 0.4% strong suppression (&lt; − 20%); 57.9% of interactions were enhancing, giving a net mean signed ME of + 3.3%. Two composite metrics were introduced: the matrix severity index (MSI), the mean absolute ME per matrix, and the matrix mitigation efficiency index (MMEI), the fraction of analytes within ± 15% of the reference under alternative injection solvents; the MSI is interpreted jointly with the mean signed ME to retain directional information. MSI ranged from 3.68 (green bean) to 10.07 (fennel), with aromatic, high-organic-matter commodities forming a high-severity cluster in principal component analysis (PCA; 77.3% of variance). A weak but significant log K<sub>ow</sub> –ME correlation (R<sup>2</sup> = 0.118, <i>p</i> = 0.0009) indicated lipophilicity as one contributory determinant (≈ 12% of variance). ACN/H₂O (10:90, v/v) was the optimal injection solvent (MMEI = 86.0%). Recovery at 100 µg kg⁻<sup>1</sup> was 100.2 ± 35.4%, with HorRat values below 0.73 confirming excellent precision; expanded uncertainty (k = 2) was below 25% for 72% of analytes under the GUM framework. The framework supports matrix-matched calibration, dilution, and uncertainty-budget decisions in regulatory food monitoring.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 6","pages":"625 - 638"},"PeriodicalIF":1.6,"publicationDate":"2026-07-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148974830","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Simplified and Sensitive Mixed-Mode SPE-Based LC-MS/MS Method for the Simultaneous Determination of Insulin Glargine and Its Metabolites M1 and M2 简化灵敏的混合模式spe - LC-MS/MS同时测定甘精胰岛素及其代谢产物M1和M2的方法
IF 1.6 4区 化学
Chromatographia Pub Date : 2026-07-02 DOI: 10.1007/s10337-026-04500-4
Sandeep Chakravarthi Kuppirala, Somasekhar Reddy Kanala
{"title":"Simplified and Sensitive Mixed-Mode SPE-Based LC-MS/MS Method for the Simultaneous Determination of Insulin Glargine and Its Metabolites M1 and M2","authors":"Sandeep Chakravarthi Kuppirala,&nbsp;Somasekhar Reddy Kanala","doi":"10.1007/s10337-026-04500-4","DOIUrl":"10.1007/s10337-026-04500-4","url":null,"abstract":"<div><p>A sensitive analytical method was developed and validated for the simultaneous quantification of insulin glargine and its active metabolites M1 and M2 in human K₂EDTA plasma. Plasma sample extraction was performed using an optimized mixed-mode solid-phase extraction (SPE) procedure, followed by analysis using liquid chromatography–tandem mass spectrometry (LC–MS/MS API 6500+) in positive electrospray ionization mode. The method specificity, linearity, sensitivity, recovery, accuracy, precision, IS-normalized matrix factor, matrix effect, and stability, were systematically validated as per ICH M10 guidelines. The method exhibited high specificity, with no significant interference at the retention times of analytes and internal standards. The calibration curves showed linearity over the concentration range of approximately 70–2200 pg/mL, with regression coefficients (r<sup>2</sup>) ≥ 0.995. The lower limit of quantification was approximately 70 pg/mL for analyte and metabolites. Observed intra-day and inter-day precision (2.93–11.27%) and accuracy were well within acceptable regulatory thresholds. The overall mean analyte recovery was consistent (61–63%) with low variability (CV &lt; 5%) across three quality control levels. Internal standard normalization method demonstrated minimal matrix effect with a %CV ≤ 7.74%. The validated method thus delivers high sensitivity and reproducible quantification while maintaining a notably simplified sample preparation workflow without the need for immunoaffinity purification (IAP). The designed and tested method is valid and applicable for pharmacokinetic, bioavailability, and bioequivalence studies of insulin glargine and its metabolites.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 6","pages":"607 - 624"},"PeriodicalIF":1.6,"publicationDate":"2026-07-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148974787","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Simultaneous Determination of Eleven Biogenic Amines via Underivatized HILIC-MS/MS Without Ion-Pairing Reagents 不使用离子配对试剂的HILIC-MS/MS同时测定11种生物胺
IF 1.6 4区 化学
Chromatographia Pub Date : 2026-06-25 DOI: 10.1007/s10337-026-04499-8
Chunyan Chen, Yu Luo, Min Zhang, Zhibin Liu, Mengyue Hu, Jinlin Li
{"title":"Simultaneous Determination of Eleven Biogenic Amines via Underivatized HILIC-MS/MS Without Ion-Pairing Reagents","authors":"Chunyan Chen,&nbsp;Yu Luo,&nbsp;Min Zhang,&nbsp;Zhibin Liu,&nbsp;Mengyue Hu,&nbsp;Jinlin Li","doi":"10.1007/s10337-026-04499-8","DOIUrl":"10.1007/s10337-026-04499-8","url":null,"abstract":"<div><p>In present research, a hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) method was proposed for the concurrent determination of 11 biogenic amines, including putrescine (PUT), cadaverine (CAD), histamine (HIS), 2-phenethylamine (2-PHE), tyramine (TYR), spermidine (SPD), octopamine (OA), 5-hydroxytryptamine (5-HT), adrenaline (A), tryptamine (TRP), and spermine (SPM) within 11 min. A Waters ACQUITY UPLC<sup>®</sup> BEH Amide (100 mm × 2.1 mm i.d., 1.7 μm) was used as stationary phase. Gradient elution was conducted using a mobile phase of 90% acetonitrile aqueous solution (10 mM ammonium formate, 0.6% formic acid) and aqueous solution (300 mM ammonium formate). This method provides symmetrical peak shapes and satisfactory separation for all the biogenic amines. Furthermore, it displays high linearity (R<sup>2</sup> &gt; 0.97) except spermine and sensitivity (LODs ≤ 3 ng/mL). Importantly, the approach is convenient, rapid, and sensitive, without derivatization or ion-pairing reagents. Thus, the proposed HILIC-MS/MS method shows significant potential for both targeted and untargeted analysis of highly charged, small polar basic organic compounds in food safety supervision, metabolomics, environmental analysis, clinical research and relevant areas.</p></div>","PeriodicalId":518,"journal":{"name":"Chromatographia","volume":"89 5","pages":"589 - 596"},"PeriodicalIF":1.6,"publicationDate":"2026-06-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"148695244","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
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