BMC Chemistry最新文献

{"title":"Determination of 229 pesticides residue in edible oil samples using conventional quechers method and solid phase microextraction based on monolithic molecularly imprinted polymer fiber and analysis with GC-MS","authors":"Fatemeh Kardani,&nbsp;Aniseh Zarei Jelyani,&nbsp;Tahere Khezeli,&nbsp;Mohammad Hashemi,&nbsp;Marzieh Rashedinia,&nbsp;Saeedeh Shariati,&nbsp;Masoud Mahdavinia,&nbsp;Seyyed Mohammad Ali Noorie","doi":"10.1186/s13065-025-01518-x","DOIUrl":"10.1186/s13065-025-01518-x","url":null,"abstract":"<div><p>The goal of this research is the development of a solid phase microextraction based on monolithic molecularly imprinted polymer fiber (SPME-MMIPF) method to determine 229 pesticides in edible oil samples using gas chromatography-mass spectrometry (GC-MS) and comparison of it with the common QuEChERS method. For SPME-MMIPF method, an MMIPF was synthesized by polymerization of methacrylic acid in presence of ethylene glycoldimethacrylate and azo (bis)-isobutyronitrile. The optimal conditions for the SPME-MMIPF method are: extraction time 30 min, desorption time with toluene 20 min and string speed of the aqueous sample 600 rpm. Under optimal extraction condition, the figures of merit were obtained for two methods and compared. The linear range of 1–300 µg kg^− 1 for SPME-MMIPF and 10–250 µg kg^− 1 for QuEChERS was obtained. The detection limits of SPME-MMIPF (0.300–0.335 µg kg^− 1) method was better than the QuEChERS (0.9–2.8 µg kg^− 1) method. The results showed a quantification limit of 0.990–1.102 µg kg^− 1 for SPME-MMIPF and 3.0–9.2 µg kg^− 1 for QuEChERS. The recoveries were in the range of 92–102% and 68–127% for SPME-MMIPF and QuEChERS, respectively.</p></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-05-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01518-x","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144125739","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Synthesis of 99mTc-labeled polyaspartic acid/silica nanoassembly as a potential probe for bone imaging","authors":"Noha A. Bayoumi,&nbsp;Marwa E. Sayyed,&nbsp;Wael M. Darwish","doi":"10.1186/s13065-025-01508-z","DOIUrl":"10.1186/s13065-025-01508-z","url":null,"abstract":"<div><h3>Purpose</h3><p>Due to the efficient bone targeting of mesoporous silica nanoparticles (MSNs) and polyaspartic acid (PASP), ^99mTc- labeled polyaspartic acid coated mesoporous silica nanoparticles (PASP-mSiO₂-DTPA-^99mTc) are proposed as a potential probe for bone imaging.</p><h3>Methods</h3><p>Polyaspartic acid-conjugated silica nanoparticles (PASP-mSiO₂) were synthesized using aqueous carbodiimide chemistry and characterized by ATR-FTR, FE-SEM, EDX, TEM, TGA and XRD. Radiolabeling of the produced nanoassembly with ^99mTc was carried out via a simple DTPA chelation procedure. Aqueous dispersion of the radiolabeled nanoparticles was intravenously injected into normal mice and the bone targeting efficiency was evaluated.</p><h3>Results</h3><p>The PASP-mSiO₂ nanoassembly was efficiently synthesized and radiolabeled with ^99mTc with a high radiochemical yield (92 ± 0.5%) and sufficient in vitro stability in PBS and FBS for up to 24 h. In vivo biodistribution studies revealed a significant enhancement of radioactivity bone uptake after intravenous injection of PASP-mSiO₂-DTPA-^99mTc compared to radiolabeled uncoated MSNs (mSiO₂-DTPA-^99mTc), (13 ± 0.6% IA/gram and 5.4 ± 0.4, respectively).</p><h3>Conclusion</h3><p>PASP endowed MSNs with enhanced biocompatibility and highly selective bone targeting. Therefore, the proposed PASP-mSiO₂-DTPA-^99mTc nanoassembly has immense potential in the field of bone- imaging via single photon emitting computed tomography (SPECT).</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div><div><p>.</p></div></div></figure></div></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-05-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01508-z","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144125741","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Structural stability of Calmodulin-target peptide complex at different temperatures based on molecular dynamics simulation","authors":"Jiayi Ding,&nbsp;Zhaoyang Ju,&nbsp;Tengfei Fu,&nbsp;Liyong Ding,&nbsp;Xinyi Yan,&nbsp;Bing Zhou,&nbsp;Mengting Yu,&nbsp;Chengsheng Ge","doi":"10.1186/s13065-025-01515-0","DOIUrl":"10.1186/s13065-025-01515-0","url":null,"abstract":"<div><p>Calmodulin (CaM) is a multifunctional protein commonly found in various eukaryotic cells that can bind Ca²⁺, making it highly valuable for research in agriculture, medicine, the environment, and other fields. Protein functionality is intricately linked to its structure. To understand how varying temperatures affect the structural integrity of CaM protein at the molecular level, the effect of temperature on the structural stability of CaM-peptide complex was investigated based on the molecular dynamics (MD) simulation. Some analyses including the root mean square deviation (RMSD) values, interaction energies, the decomposition of total energy of the system, the binding mechanism for Ca²⁺, and the secondary structure of CaM-peptide at different temperatures have been made in this work. The RMSD increased from 0.5277 nm (298 K) to 0.6949 nm (400 K), indicating a loss of structural stability. As temperature increases, the interaction energies between CaM-peptide and Ca²⁺ exhibit a decline, and the number of oxygen atoms in the 4 Å range around the CaM-peptide ion tends to decrease, with the average value of the number of oxygen atoms in the 4 Å range of CaM-peptide decreasing from 7.48039 (298 K) to 6.36614 (400 K) with Coulombic interactions playing a pivotal role in stabilizing Ca²⁺. This decline in hydrogen bonding is directly linked to a decrease in protein stability at higher temperatures, highlighting the thermal sensitivity of the protein’s structural framework. The stable secondary structures, including the α-helix, are disrupted as temperatures increase, leading to the gradual unwinding of the α-helix and a loss of structural integrity. This work explores the molecular-level structural stability of CaM, enhancing our understanding of CaM protein and its potential applications.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-05-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01515-0","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144125740","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Cutting-edge assays for mirabegron and tadalafil combo therapy for benign prostatic hyperplasia; insilico kinetics approach; multi trait sustainability assessment","authors":"Sara I. Aboras,&nbsp;Mohamed R. Abdelhakim,&nbsp;Hadir M. Maher,&nbsp;Rasha M. Youssef","doi":"10.1186/s13065-025-01497-z","DOIUrl":"10.1186/s13065-025-01497-z","url":null,"abstract":"<div><p>The combination therapy of mirabegron (MIR) and tadalafil (TAD) has gained significant attention in clinical practice for the treatment of Benign Prostatic Hyperplasia as well as overactive bladder syndrome. This study demonstrates the development and validation of two analytical methods for the concurrent determination of tadalafil and mirabegron in their synergistic combo therapy. Spectrophotometry and stability-indicating HPLC were employed for the accurate quantification of both drugs. The spectrophotometric methods were based on derivative, Fourier and ratio derivative of the two drugs, providing simpler, rapid alternatives for routine analysis. The stability-indicating HPLC method was developed using a reverse-phase column with a methanol-phosphate buffer gradient mobile phase, achieving optimal separation with detection at 250 nm for MIR and 225 nm for TAD. Forced degradation studies were performed under acidic, basic, oxidative, neutral, thermal, and photolytic conditions, confirming the method’s ability to quantify MIR and TAD in presence of degradation products and establish drug stability. Both techniques were validated based on ICH guidelines, demonstrating excellent linearity, precision, accuracy, and sensitivity. The methods were successfully applied to the analysis of bulk powder and in dosage forms. Both methods were evaluated and found to be environmentally friendly, receiving approval as “green” according to the AGREE (Assessment Tool for Greenness) method, “white” under the RGB12 criteria, and “blue” according to the BAGI (Blue Analytical Greenness Index). These evaluations demonstrate the sustainability and eco-friendliness of the proposed analytical techniques. Furthermore, artificial intelligence was employed through an online tool to ensure that there were no potential drug-drug interactions between MIR and TAD, offering an additional layer of safety in clinical applications. This research contributes to the enhancement of quality control for patients undergoing combination therapy with MIR and TAD and stability testing.</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-05-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01497-z","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144117637","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"An eco-friendly bioanalytical RP-HPLC method coupled with fluorescence detection for simultaneous estimation of felodipine and metoprolol","authors":"Mariam Wasim Beniamin,&nbsp;Amira Mohamed Kessiba,&nbsp;Maha Abdelmonem Hegazy,&nbsp;Ahmed Emad El Gendy,&nbsp;Lubna Ahmed Kormod","doi":"10.1186/s13065-025-01507-0","DOIUrl":"10.1186/s13065-025-01507-0","url":null,"abstract":"<div><p>An ecofriendly, sensitive, selective, precise, and accurate HPLC method with fluorescence detection (FD) has been developed and validated for simultaneous determination of two hypertensive drugs, felodipine and metoprolol in their pure samples, combined pharmaceutical dosage form and in spiked human plasma. Separation was carried out on Inertsil C₁₈ column (150 mm × 4.6 ID; Particle size 5 µm) and a mobile phase composed of ethanol and 30mM potassium dihydrogen phosphate buffer, adjusted to pH 2.5 using ortho-phosphoric acid (40:60, v/v) was used. A constant flow rate of 1.0 mL/min at an ambient temperature was adopted. Method validation was performed according to the ICH Q2 R2 and bioanalytical method validation was done according to FDA guidelines for determination of both drugs simultaneously in biological matrices. The method demonstrated excellent linearity over the concentration range of 0.01–1.00 µg/mL and 0.003–1.00 µg/mL that were selected with accordance to the C_max of both drugs with a correlation coefficient (r²) of 0.9998 and 0.9999 for felodipine and metoprolol, respectively in human plasma. The intra-day and inter-day precision were ≤ 2% in their pure forms and in spiked human plasma, and the accuracy was within ± 2% of the nominal concentration for both drugs in their pure forms and within ± 10% of the nominal concentration in human plasma. A statistical comparison was conducted between the proposed method and the reported method; it showed no significant difference between both methods regarding both accuracy and precision. The proposed method proved to be eco-friendly with three green assessment tools (AGREE calculator, MoGAPI, RGBfast study).</p><h3>Graphical Abstract</h3><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-05-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01507-0","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144125524","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Molecular hydrogen mitigates traumatic brain injury-induced lung injury via NLRP3 inflammasome inhibition","authors":"Lingling Liu,&nbsp;Shuzhi Wang,&nbsp;Lianhao Jiang,&nbsp;Jiwei Wang,&nbsp;Jun Chen,&nbsp;Hongtao Zhang,&nbsp;Yuanlin Wang","doi":"10.1186/s13065-025-01513-2","DOIUrl":"10.1186/s13065-025-01513-2","url":null,"abstract":"<div><h3>Introduction</h3><p>Hydrogen gas has demonstrated significant antioxidant and anti-inflammatory properties, suggesting potential therapeutic benefits in TBI.</p><h3>Methods</h3><p>We subjected to controlled cortical impact in mice to construct TBI model. They received an intraperitoneal injection of MCC950, a selective NLRP3 inhibitor, at 10 mg/kg 30 min before TBI. Inhalation of 2% H₂ is adopted in TBI mice for 60 min, starting 1 and 6 h post-TBI. 24 h after H₂ inhalation, we extracted tissues and analyzed injury related changes. The H₂ levels in arterial and venous were tracked after inhalation. Lung tissue was examined for histopathological changes and apoptosis using H&amp;E and TUNEL assays. The total protein in the BALF, oxygenation index, lung wet-to-dry weight ratio, and lung MPO activity were measured to evaluate the severity of TBI-induced lung injury. Protein and mRNA levels of NLRP3, ASC, Caspase-1, IL-18, and IL-1β in the lung tissue were quantified using western blotting and quantitative PCR. The expression changes and distribution status of NLRP3 and Caspase-1 were examined by immunofluorescence and immunohistochemistry staining.</p><h3>Results</h3><p>Significant lung injury at 24 h post-TBI got significantly reduced by treatment of 2% H₂. TBI activated the NLRP3 inflammasome, increasing NLRP3, ASC, and caspase-1 levels, to lead to higher IL-1β and IL-18 secretion in the lungs. Blocking NLRP3 reduced lung damage from TBI, and its combination with 2% H₂ provided better protection than either treatment alone.</p><h3>Conclusions</h3><p>2% H₂ can protect against TBI-induced lung injury by inhibiting NLRP3 inflammasome activation, thereby alleviating inflammation and inhibiting apoptosis.</p></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01513-2","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144117785","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Synthesis and characterization of glyoxal-crosslinked chitosan with N-amino anthracene succinimide polymers for antimicrobial applications","authors":"Ahmed G. Taha,&nbsp;A. M. Hezma","doi":"10.1186/s13065-025-01505-2","DOIUrl":"10.1186/s13065-025-01505-2","url":null,"abstract":"<div><p>This paper presents the synthesis and characterization of a novel chitosan-derivative polymers by using glyoxal as acrosslinker between chitosan and N-amino-9,10-dihydro-anthracene-9,10-α,β-succinamide (AS) under our conditions. The generated polymers were characterized using X-ray diffraction (XRD) and infrared spectroscopy (IR). The results indicate the successful formation of new polymer structures with unique properties. The antimicrobial activity of Chs-Gly-AS and its modified derivatives was evaluated using the cup diffusion agar method, showing enhanced inhibition against bacteria and fungi. The results demonstrate promising antimicrobial efficacy, suggesting the potential use of these polymers in antimicrobial applications.</p></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01505-2","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144117554","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Engine performance and emission optimization with waste cooking oil biodiesel/diesel blend using ANN and RSM techniques coupled with ACKTR-DE and HHO algorithms","authors":"Mehmet Ali Biberci,&nbsp;Mustafa Bahattin Çelik,&nbsp;Esma Ozhuner","doi":"10.1186/s13065-025-01512-3","DOIUrl":"10.1186/s13065-025-01512-3","url":null,"abstract":"<div><p>In this experimental investigation, Artificial Neural Network (ANN) and Response Surface Methodology (RSM) model structures were constructed to predict and optimize the performance and exhaust emissions of a diesel engine operating on a blend of diesel fuel and waste oil biodiesel. The test engine was operated with 0%, 50%, and 100% biodiesel content under varying injection pressures and loads. The RSM model was used to derive regression equations from the experimental results. The correlation coefficient (R²) for all responses of the constructed model ranged from 0.9785 to 0.9997. By applying the developed model, the brake thermal efficiency (BTE) response was optimized to its maximum value, while all other responses were minimized. All responses were predicted using an ANN model with R &gt; 0.99 and a maximum mean absolute error (MAAE) of 1.723%. RSM-based optimization analysis was applied to the design of experiments (DOE). At an injection pressure of 180 bar, an engine torque of 3.846 Nm, and a 100 percent biodiesel ratio, optimal diesel engine performance characteristics, the lowest exhaust emissions, and the lowest specific fuel consumption values were achieved. In addition, the RSM approach performed satisfactorily, with a desirability value of 0.750. The RSM regression equations were assessed using the Actor Critic with Kronecker-Factored Trust Region-Differential Evolution (ACKTR-DE) and Harris Hawks Optimization (HHO) algorithms. The outcomes derived from the ACKTR-DE and HHO algorithms corroborated the results obtained from the RSM. Furthermore, verification experiments were conducted to confirm the optimal results, thus demonstrating that the combined use of RSM, ANN, and advanced algorithms offers a robust and accurate framework for optimizing biodiesel engine performance.</p><h3>Graphical Abstract</h3>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01512-3","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144117786","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Green chromatographic approach to determine methocarbamol, aspirin and their related impurities in their combined pharmaceutical formulation and human plasma: with computational evaluation","authors":"Yasmine F. Bassuoni,&nbsp;Asmaa M. AboulMagd,&nbsp;Maha M. Ibrahim","doi":"10.1186/s13065-025-01500-7","DOIUrl":"10.1186/s13065-025-01500-7","url":null,"abstract":"<div><p>Nowadays, one of the main objectives is to protect the environment and reduce the adverse impacts of chemicals on it. One of the most difficult issues for researchers is determining the efficiency and quality of the suggested approach in terms of environmental and human safety. The present research presents advanced, accurate, green high-performance liquid chromatographic method (HPLC) to estimate a combination of methocarbamol (MET) and aspirin (ASP) as well as their related impurities, guaifenesin (GUF) and salicylic acid (SA), respectively, with low retention time and ideal separation. Chromatographic separation was performed on X-Bridge C₈ reversed phase (RP) column (4.6 × 250 mm, 5 μm particle size) utilizing methanol: water: triethylamine (70:30, 0.1% by volume) at pH 3.00 by o-phosphoric acid as a mobile phase with 2.00 mL min⁻¹ flow rate at 254.00 nm. The proposed method succeeded to achieve linearity over a concentration ranges of 0.30–50.00 μg mL⁻¹, 1.00–300.00 μg mL⁻¹, 10.00–500.00 μg mL⁻¹ and 0.10–50.00 μg mL⁻¹ for GUF, MET, ASP and SA, respectively. All the developed results were validated in compliance with the International Council of Harmonization (ICH) instructions. The suggested method was successfully applied to assess MET and ASP in their pharmaceutical formulation and in spiked human plasma. The molecular docking approach was employed to evaluate how the two drugs and their related impurities interacted with the stationary phase and to predict the suggested sequence of elution. The greenness of the developed analytical method was evaluated using whiteness assessment and two green approaches; analytical eco-scale and AGREE. The proposed method proved not only to be green, time-saving and more sensitive for the routine analysis of MET and ASP in QC laboratories, but also it can effectively handle the presence of impurities such as GUF and SA.</p><h3>Graphical Abstract</h3>\u0000<div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-05-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01500-7","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144100328","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Green and sustainable LC-APCI-MS/MS method for simultaneous quantification of genotoxic nitrosamines in antidiabetic medication: sitagliptin","authors":"Sriram Pepakayala,&nbsp;Venkata Nadh Ratnakaram,&nbsp;Yuvaraj Zunjarrao,&nbsp;Yogesh Kumar Lohia","doi":"10.1186/s13065-025-01503-4","DOIUrl":"10.1186/s13065-025-01503-4","url":null,"abstract":"<p>The International Agency for Research on Cancer categorized nitrosamines as potential or probable human carcinogens. Hence, nitrosamine impurities should be controlled to minimize the cancer risk. Sustainable Development Goal 9 (SDG9: Industry, Innovation, and Infrastructure), Target 9.4 was realized by developing a simple and straightforward LC-APCI-MS/MS method for simultaneous determination of potential nitrosamines: N-nitroso dimethylamine, N-nitroso di isopropyl amine, N-nitroso isopropyl ethylamine and N-nitroso methyl aminopyridine (NDMA, NDIPA, NIPEA and NMAP) in Sitagliptin Phosphate Monohydrate API (STG-API), an antidiabetic medication for type-2 diabetes and validated as per ICH (Q2 R2) guidelines. As a part of SDG9 (Industry, Innovation, and Infrastructure), Target 9.4, greater adoption of clean and environmentally sound technologies is possible by using the current analytical method in view of (a) less consumption of solvents as it has a lower run time of 18 min (b) at-line sample collection (c) simple sample preparation (d) sample preparation process that does not require derivatization or sample extraction. The optimized LC method conditions are an Agilent Poroshell EC C18 column, a flow rate of 0.6 mL/min, an injection volume of 40 µL, a column oven temperature set at 50 °C, and a sample cooler temperature set at 6 °C. A gradient method was adopted using a mixture of mobile phases (Solvent A: 0.1% formic acid in water and Solvent B: a mixture of 50% Methanol and 50% Acetonitrile). The response was obtained with Multiple Reaction Monitoring (MRM) in APCI mode. The current method can quantify NDMA, NIPEA, NDIPA, and NMAP to a lower level of 74.19 ng/g, 19.62 ng/g, 20.36 ng/g, and 13.65 ng/g, respectively, which is less than 10% of the specified limits. Good linearity in the range of Limit of Quantitation (LOQ) to 150% of the specification limit was observed, with correlation coefficients higher than 0.996. The recoveries were over the range between 90.23 and 103.36%. Assessed the method’s eco-friendliness by greenness tools like the Modified Green Analytical Procedure Index (MoGAPI), ComplexMoGAPI, Analytical GREEnness (AGREE), and Analytical Eco-Scale, and found it to be eco-friendly.</p>","PeriodicalId":496,"journal":{"name":"BMC Chemistry","volume":"19 1","pages":""},"PeriodicalIF":4.3,"publicationDate":"2025-05-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://bmcchem.biomedcentral.com/counter/pdf/10.1186/s13065-025-01503-4","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144100309","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}