Journal of Applied Spectroscopy最新文献

{"title":"Development and Validation of a High-Sensitivity HPLC Method for Quantification of Ketoconazole: Ensuring Quality Assurance Through Specific Chromatographic Procedures","authors":"Nishant Gaur,&nbsp;Nayyar Parvez,&nbsp;Kalpana Nagpal","doi":"10.1007/s10812-025-01929-7","DOIUrl":"10.1007/s10812-025-01929-7","url":null,"abstract":"<p>Analyzing the drug substance serves as a crucial step in verifying the quality of the active pharmaceutical ingredient. This research is aimed at developing an isocratic high-performance liquid chromatography (HPLC) method for the quantitative analysis of ketoconazole in its stable form. The novelty of this work lies in its remarkable specificity and sensitivity, ensuring highly accurate results. Chromatographic separation was performed using an Xterra RP C18 column (250 × 3.0 mm) with a particle size of 5 μm, and detection was carried out with UV at 244 nm. The sequence run time was 8 min, with the average analyte peak eluting at 3.469 min while maintaining a flow rate of 1.0 mL/min. The preparation of both the sample and the mobile phase is rapid and highly economical, significantly reducing the chances of manual error. The analysis duration has been notably reduced to approximately 8 min, with the analyte eluting in under 5 min. This represents a significant improvement in efficiency compared with earlier reports. The method performance was validated following the current International Conference on Harmonization (ICH) guidelines, covering aspects such as specificity, system suitability, limits of detection (LOD) and quantification (LOQ), linearity, accuracy, and precision. Regression analysis revealed a correlation coefficient value of 0.9982. The LOD and LOQ were found to be 10 and 30 μg/mL respectively. The accuracy of the method was evaluated through a recovery study at levels of 80, 100, and 120%, and the values were found to be within the acceptable range (% relative standard deviation [RSD] less than 2%). The RSD for method precision experiments was found to be 1.0%, which complies with the ICH guidelines. This method was successfully developed for the estimation of ketoconazole using a straightforward and effective isocratic technique.</p>","PeriodicalId":609,"journal":{"name":"Journal of Applied Spectroscopy","volume":"92 2","pages":"437 - 445"},"PeriodicalIF":1.0,"publicationDate":"2025-05-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145171518","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}

{"title":"Green Analytical Chemistry Compliant UV-Visible Spectrophotometry Estimations for Sunitinib Malate","authors":"Gaurav G. Patil,&nbsp;Rucha S. Bhave,&nbsp;Preeti S. Bobade,&nbsp;Darshan R. Telange,&nbsp;Saurabh B. Ganorkar,&nbsp;Atul. A. Shirkedkar","doi":"10.1007/s10812-025-01930-0","DOIUrl":"10.1007/s10812-025-01930-0","url":null,"abstract":"<p>Sunitinib malate (SNM), a vital antineoplastic drug, needed a greener and more rapid spectrophotometric method for its pharmaceutical quantification. This study involves developing and validating two effective and environmentally friendly ultra-violet-visible (UV-Vis) spectrophotometric methods for measuring SNM in bulk form and capsule formulations produced in-house. These methods were developed using the zero-order UV-Vis spectrophotometry (method I) and area under the curve (UV-Vis–AUC) (method II) approaches. The method sensitivities and selectivity were optimized using ethanol as a green solvent, which was not found to be reported before for estimation of SNM. Both devised methods underwent validation to ensure precision, accuracy, and sensitivity to comply with the International Council for Harmonization Q2 R1 guideline. SNM was formulated as in-house capsules using microcrystalline cellulose. The validated methods were used to estimate SNM as a bulk assay from in-house capsules. The results demonstrated excellent Beer–Lambert linearity within 3–18 μg/mL with acceptable accuracy and adequate precision. The limit of detection (LOD) (method I: 0.43 μg; method II: 0.15 μg) and limit of quantification (LOQ) (method I: 1.32 μg; method II: 0.45 μg) values confirmed the method's sensitivity. Additionally, the method exhibited exceptional specificity and was free from interferences from used excipients. This newly developed UV-spectrophotometric method complies with principles for green analytical chemistry as assessed with the Analytical Greenness Assessment (AGREE) tool and was found to be rapid, simple, cost-effective, and reliable for the routine analysis of SNM to assist with its pharmaceutical research in the future.</p>","PeriodicalId":609,"journal":{"name":"Journal of Applied Spectroscopy","volume":"92 2","pages":"446 - 454"},"PeriodicalIF":1.0,"publicationDate":"2025-05-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145171524","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}

{"title":"Photosensitive Polymer Material for Volume and Relief Phase Holographic Recording in a Wide Spectral Range","authors":"U. V. Mahilny,&nbsp;D. E. Stasevich,&nbsp;E. A. Khramtsou,&nbsp;A. P. Shkadarevich","doi":"10.1007/s10812-025-01915-z","DOIUrl":"10.1007/s10812-025-01915-z","url":null,"abstract":"<p>The phase response of a new polymer with anthracene side-groups was shown experimentally to be created by their photooxidation and photodimerization. Both photoreactions lead to approximately equal photorefraction in the volume of the material (∆<i>n</i> ≈ –0.02 for λ = 633 nm) and formation of a photorelief on the layer surface. Estimation of the refractive index modulation depth in the structure of the two-dimensional holographic gratings indicates the possibility of achieving maximum diffraction efficiency, which is limited for three-dimensional gratings by their nonsinusoidality. This polymer and its compositions with various photosensitizers in thin (~1 μm) layers were shown to effectively form surface photoreliefs with spatial frequency up to 1000 mm^–1 and amplitude up to 25% of the layer thickness when using post-exposure reversible plasticization. Our experiments showed that the resistance of the surface reliefs to the action of temperatures above 90oC can be increased manyfold by photocross-linking the material of the formed relief material.</p>","PeriodicalId":609,"journal":{"name":"Journal of Applied Spectroscopy","volume":"92 2","pages":"321 - 328"},"PeriodicalIF":1.0,"publicationDate":"2025-05-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145171517","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}

{"title":"Using a Probability Generating Functional for Analysis of Photon Arrival Processes in Single-Quantum Registration Systems of Fluorescence Intensity","authors":"V. V. Skakun,&nbsp;V. V. Apanasovich","doi":"10.1007/s10812-025-01914-0","DOIUrl":"10.1007/s10812-025-01914-0","url":null,"abstract":"<p>An expression for the probability generating functional of photon arrival processes in fluorescence fluctuation spectroscopy systems assuming an arbitrary fluorescence intensity over the observation interval is obtained. The use of generating functionals generalizes the theory of photon counting distribution analysis methods based on the application of photon counts generating functions and opens the possibility of analyzing systems with nonstationary intensity over the observation interval. Expressions for the process intensity and the probability of obtaining a certain number of photocounts per observation interval are found. Based on the obtained expressions, a method for estimating the concentration of fluorescent molecules with an arbitrary fluorescence intensity is developed. The method is applicable for both single-photon and two-photon excitation and does not depend on the form of the brightness profile function.</p>","PeriodicalId":609,"journal":{"name":"Journal of Applied Spectroscopy","volume":"92 2","pages":"309 - 320"},"PeriodicalIF":1.0,"publicationDate":"2025-05-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145171525","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}

{"title":"Nonlinear Interaction of q-Gaussian Laser Beam with Unmagnetized Plasma: Effect of Relativistic and Ponderomotive Nonlinearity","authors":"Keshav Walia,&nbsp;Anamika Tripathy","doi":"10.1007/s10812-025-01917-x","DOIUrl":"10.1007/s10812-025-01917-x","url":null,"abstract":"<p>The present work explores the nonlinear interaction of <i>q</i>-Gaussian laser beam with unmagnetized plasma. Relativistic and ponderomotive nonlinearities are taken together in the present investigation. The Wentzel–Kramers–Brillouin (WKB) approximation and paraxial theory are used for deriving the second-order ODEexpressing variation of beam waist against the normalized propagation distance. Further, the behavior of the beam waist against normalized propagation distance is explored through the RK4 method. The impact of established parameters of laser and plasma such as plasma temperature, laser intensity, plasma density, and q parameter on the beam waist is also analyzed.</p>","PeriodicalId":609,"journal":{"name":"Journal of Applied Spectroscopy","volume":"92 2","pages":"335 - 341"},"PeriodicalIF":1.0,"publicationDate":"2025-05-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145171516","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}

{"title":"X-Ray Absorption Fine Structure Study of Mixed Ligand Pyridine Octahedral Co(II) Complexes Having Axial Compressed/Elongated Distortion","authors":"S. Dubey,&nbsp;M. Bairagi,&nbsp;P. Sharma,&nbsp;A. Mishra,&nbsp;P. K. Sharma,&nbsp;B. D. Shrivastava,&nbsp;S. N. Jha,&nbsp;D. Bhattacharya","doi":"10.1007/s10812-025-01918-w","DOIUrl":"10.1007/s10812-025-01918-w","url":null,"abstract":"<p>X-ray absorption fine structure (XAFS) at the Co K-edge in three mixed ligand pyridine Co(II) complexes, viz., [Co(py)₄(SCN)₂] (<b>1</b>), [Co(py)₄(Cl)₂]∙H₂O (<b>2</b>), and [Co(py)₄(Br)₂] (<b>3</b>), have been investigated using synchrotron radiation. Extended X-ray absorption fine structure (EXAFS) has been analyzed using two methods to present their comparative study. In the first method, the coordination number <i>N</i> is fixed, and the amplitude reduction factor <span>({S}_{0}^{2})</span> is varied. In the second method, <i>N</i> is varied and <span>({S}_{0}^{2})</span> is fixed. EXAFS analysis indicated that the absorbing Co atom is surrounded by four <i>N</i> atoms (of pyridine ligands) in the equatorial positions forming the square planar base. Two <i>N</i> atoms (of thiocyanate), two chlorides, and two bromide ions in the axial sites complete the distorted octahedral coordination in complexes <b>1</b>, <b>2</b>, and <b>3</b>, respectively. Whereas in <b>1</b>, the axial bond lengths are shorter than the equatorial bond lengths, indicating compressed octahedral geometry, in <b>2</b> and <b>3</b> the axial bond lengths are longer than the equatorial bond lengths, exhibiting elongated octahedral geometry. The results agree with those obtained previously using X-ray crystallography. Using ab initio calculations, X-ray absorption near edge structure (XANES) spectra have been simulated and compared with the experimental XANES spectra. Further, <i>p</i>- and d-DOS calculated simultaneously to absorb the metal center of Co have been correlated with the features and shapes of the simulated XANES spectra, as well as the experimental spectra.</p>","PeriodicalId":609,"journal":{"name":"Journal of Applied Spectroscopy","volume":"92 2","pages":"342 - 351"},"PeriodicalIF":1.0,"publicationDate":"2025-05-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145171822","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}

{"title":"Validated Stability-Indicating Method Development Designed for the Determination of Metronidazole in the Presence of Povidone-Iodine in Dermatological Formulation by a First-Order Derivative UV Spectrophotometric Method","authors":"Pratiksha Fulzele,&nbsp;Swati Pandey,&nbsp;Ravindra Pandey,&nbsp;Shiv Shankar Shukla","doi":"10.1007/s10812-025-01928-8","DOIUrl":"10.1007/s10812-025-01928-8","url":null,"abstract":"<p>Metronidazole, a nitroimidazole antimicrobial, is used in combination with povidone iodine in the form of a topical ointment for treating and preventing skin infections in several skin conditions such as otitis externa, sycosis barbae, tinea infestations, cutaneous candidosis, burns, boils, or ulcers. The study presented is aimed at developing a stability-indicating method for the determination of metronidazole in the presence of povidone-iodine in dermatological formulations by a first-order derivative UV spectrophotometric method that provides an enhanced resolution of overlapping spectra. The λ_max was found at 319 nm for metronidazole and at 235 nm for povidone-iodine. First-order detection wavelength has been taken at 298 and 221 nm for metronidazole and povidone-iodine, respectively. Beer's law was obeyed in a concentration range of 5–45 μg/mL with R² values of metronidazole and povidone of 0.999 and 0.9967, respectively, using distilled water as an economical solvent. The developed method was validated on various parameters such as accuracy, precision, robustness, limit of quantification and limit of detection. It can be perceived from the results that a minimum intraday and interday variation limiting below 2% of relative standard deviation was established. The percentage recovery using the stated method was worthy of characteristics with its label claim and found within the range 100.22–101%, within the acceptable limits of International Conference on Harmonization guidelines for the forced degradation and establishes a validated method for metronidazole and povidone-iodine and its main degradants in the active pharmaceutical ingredients (API) and the marketed formulations. The exclusivity of the presented first-order derivative UV spectroscopic method lies in it being simple, economical, safe, precise, accurate, and reproducible for future studies of the prediction of stability of the drugs in the marketed formulation. The technique is established to be unambiguous for the determination of a drug and its degradants.</p>","PeriodicalId":609,"journal":{"name":"Journal of Applied Spectroscopy","volume":"92 2","pages":"426 - 436"},"PeriodicalIF":1.0,"publicationDate":"2025-05-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145171021","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}

{"title":"High-Temperature Raman Spectroscopy Study of the in situ Interaction Between Lanthanum Oxide and FLiNaK Fluoride Melt","authors":"I. D. Zakiryanova,&nbsp;P. N. Mushnikov","doi":"10.1007/s10812-025-01904-2","DOIUrl":"10.1007/s10812-025-01904-2","url":null,"abstract":"<p>An in situ Raman spectroscopy study has established a chemical mechanism for the interaction of lanthanum oxide with a molten fluoride mixture, FLiNaK, which holds promise for use in molten salt nuclear reactors. Hightemperature spectral studies along with the use of x-ray phase analysis and thermodynamic modeling have indicated an irreversible heterogeneous reaction La₂O_3s + 2LiF_sol → 2LaOF_s + Li₂O_sol. The reaction product in this fluoride system (lanthanum oxyfluoride, LaOF) has been shown to form hexagonal (R3m) and tetragonal (P4/nmm) crystal modifications. Data were obtained on the thermal behavior of the vibrational modes of lanthanum oxide La₂O₃ in the range 20–600oC and its interaction with atmospheric water vapor.</p>","PeriodicalId":609,"journal":{"name":"Journal of Applied Spectroscopy","volume":"92 2","pages":"249 - 255"},"PeriodicalIF":1.0,"publicationDate":"2025-05-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145171392","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}

{"title":"Simultaneous Detection of Imidacloprid, Acetamiprid, and Clothianidin in Apple Juice Using Ultraviolet Spectroscopy and the SSA–BPNN Model","authors":"Delong Meng,&nbsp;Xiaolei Yu,&nbsp;Lingyun Xu,&nbsp;Weichun Zhang,&nbsp;Zhimin Zhao","doi":"10.1007/s10812-025-01921-1","DOIUrl":"10.1007/s10812-025-01921-1","url":null,"abstract":"<p>The extensive use of pesticides can pose potential risks to food safety and human health. Therefore, establishing simple and effective detection methods for pesticide residues is necessary. In this study, ultraviolet (UV) spectroscopy is used for the simultaneous detection of imidacloprid, acetamiprid, and clothianidin in apple juice. A total of 84 samples with different concentrations of imidacloprid, acetamiprid, and clothianidin in apple juice are prepared, and the corresponding UV spectra are collected using a UV-visible spectrophotometer. The quantitative detection model is built using the back propagation neural network (BPNN), and the BPNN model is optimized using the sparrow search algorithm (SSA). To verify the performance of the model, the prediction results of the SSA−BPNN model are compared with those of the extreme learning machine (ELM), BPNN, and particle swarm optimization back propagation neural network (PSO–BPNN) models. The results show that UV spectroscopy coupled with the SSA–BPNN model is effective for the simultaneous detection of imidacloprid, acetamiprid, and clothianidin in apple juice; this method is important for ensuring food safety and human health.</p>","PeriodicalId":609,"journal":{"name":"Journal of Applied Spectroscopy","volume":"92 2","pages":"363 - 369"},"PeriodicalIF":1.0,"publicationDate":"2025-05-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145171393","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}

{"title":"Analysis of Telmisartan Using UV Spectroscopy in Marketed Samples Post Shelf-Life","authors":"Sheeja Velayudhan Kutty,&nbsp;M. A. Fasna,&nbsp;Nesiya Kunnath Hamsa,&nbsp;C. Abdul Shukoor,&nbsp;T. I. Muhamad Ajmal,&nbsp;Jikhila Machado,&nbsp;G. Megha,&nbsp;V. Divya","doi":"10.1007/s10812-025-01922-0","DOIUrl":"10.1007/s10812-025-01922-0","url":null,"abstract":"<p>This study used UV-visible spectroscopy to investigate the effectiveness of telmisartan tablets after their shelf life, employing the solubility of the drug in methanol and subsequent dilution with water to obtain an absorption maximum at 297 nm. At concentrations ranging from 0.8–4 μg/mL, the study complied with the Beer–Lambert law, and regression analysis revealed a strong correlation coefficient of 0.999. The suggested technique was found to be easy to follow, accurate, precise, and specific when applied to the analysis of tablet formulations. The developed method was validated. To study the post-shelf-life efficacy of telmisartan tablets utilizing two different brands of marketed tablets, the developed technique was followed. The results show that both expired and unexpired telmisartan tablets continue to be useful after their shelf life. The preliminary dissolution tests were performed on an electro-lab dissolution tester at 37°C. The results of the analysis showed no appreciable change in the drug concentration, suggesting that the telmisartan tablet formulation might be stable over time. The percentage release of unexpired tablets observed in the test was 99%, whereas the percentage of expired tablets was 90%.</p>","PeriodicalId":609,"journal":{"name":"Journal of Applied Spectroscopy","volume":"92 2","pages":"370 - 377"},"PeriodicalIF":1.0,"publicationDate":"2025-05-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145171688","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}