Methods and Objects of Chemical Analysis最新文献

{"title":"Speciation of Sulfamethoxazole in Pharmaceuticals via Ni(II) Complexation by Coupled CPE–LIE Techniques","authors":"Farah Abdul Adheem Razooqi, Safa Majeed Hameed","doi":"10.17721/moca.2025.123-127","DOIUrl":"https://doi.org/10.17721/moca.2025.123-127","url":null,"abstract":"A sensitive, simple, and efficient spectrophotometric method was developed for the determination of sulfamethoxazole (SMX) in pure and pharmaceutical formulations. The approach employs liquid ion exchange based on the formation of an ion-pair complex between SMX and nickel(II) ions in an acidic hydrochloric acid medium, combined with cloud point extraction (CPE) using nonionic surfactants Triton X-114 and Tween 80. Systematic optimization identified maximum absorbance wavelengths at 277 nm for Triton X-114 alone and at 291 nm for the surfactant mixture (Triton X-114 + Tween 80). Optimal extraction conditions included 0.5 M HCl, Ni²+ concentration of 100 μg mL-¹, extraction temperatures of 75°C (Triton X-114) and 80°C (surfactant mixture), and a heating duration of 15 min. Reaction kinetics evaluated via the initial rate method demonstrated rapid and efficient complex formation. The linear calibration curves ranged from 10 to 100 μg mL-¹, with limits of detection (LOD) and quantification (LOQ) of 13.3 μg mL-¹ and 40.4 μg mL-¹ (Triton X-114) and 13.4 μg mL-¹ and 40.6 μg mL-¹ (surfactant mixture), respectively. The proposed method is straightforward, reliable, and suitable for routine analysis, offering practical utility for quality control in pharmaceutical laboratories.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"20 1","pages":"123-127"},"PeriodicalIF":0.0,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"http://www.moca.net.ua/25/moca_2025_20(2)_123-127w.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147333395","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Systematic Review and Guidelines for Management of Scrotal Inguinal Hernias.","authors":"Hanh Minh Tran, Ian MacQueen, David Chen, Maarten Simons","doi":"10.3389/jaws.2023.11195","DOIUrl":"10.3389/jaws.2023.11195","url":null,"abstract":"<p><p><b>Introduction:</b> Of the more than 20 million patients undergoing groin hernia repair annually worldwide, 6% are scrotal hernias in high resource countries rising to 67% in low resource countries which represents a heavy disease burden on relatively young men during their most productive period of life. There are many open questions concerning management of scrotal hernia. These guidelines aim to improve the care for scrotal hernia patients by reducing recurrence rates, chronic pain and infection. <b>Methods:</b> After developing 19 key questions a systematic literature review was performed till 31 March 2021 for all relevant publications with search terms related to Scrotal Hernia. The articles were scored by all co-authors according to Oxford, SIGN and Grade methodologies. Statements and recommendations were formulated. Online Consensus meetings with 25 HerniaSurge members were organised with voting and grading Recommendations as \"strong\" (recommendations) or \"weak\" (suggestions) and by consensus, in some cases upgraded. <b>Results:</b> Only 23 articles (two level 2 registry and 21 level 3-5) were selected. It is proposed to define scrotal hernia as an inguinal hernia which has descended into and causes any scrotal distortion. A new classification for scrotal hernias was proposed based on hernia size, SI for upper third thigh, SII for middle thigh and SIII for lower third thigh or below. Irreducibility is denoted with IR. Despite weak evidence antibiotic prophylaxis is recommended. Urinary catheterization is recommended (upgraded) in complex cases (S2-3) due to prolonged operative time. Scrotal hernia repairs have higher associated morbidity and mortality compared to non-complex groin hernia repairs irrespective of surgical experience. Open anterior (mesh) approach is commonest technique and suture techniques in low resource countries. For minimally invasive approaches, TAPP resulted in less conversion to open approach compared to TEP. <b>Conclusion:</b> Although the evidence is scarce and often low quality scrotal hernia management guidelines aim to lead to better surgical outcomes irrespective of where patients live. This necessarily means a more tailored approach based on available resources and appropriate skills. The guidelines provide an impetus for future research where adoption of proposed classification will enable more meaningful comparison of different techniques for different hernia sizes.</p>","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"1 1","pages":"11195"},"PeriodicalIF":0.0,"publicationDate":"2023-03-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10831669/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89550851","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Development, Optimization, and Validation of a Novel HPLC Method for Simultaneous Quantification of Artesunate and Amodiaquine in Tablet Formulations","authors":"Fouad Echerfaoui, H. Bouchafra, K. El Bourakadi, A. El Orche, Mounir El Kacemi, Abdelhafid Benomar, K. Karrouchi, M. Bouatia, M. El Karbane","doi":"10.17721/moca.2023.42-50","DOIUrl":"https://doi.org/10.17721/moca.2023.42-50","url":null,"abstract":"Artemisinin-based combination therapy (ACTs) has become the primary first-line treatment for mild falciparum malaria in the majority of African countries. A fixed-dose combination of amodiaquine and artesunate is commonly employed to enhance treatment compliance and achieve successful malaria outcomes. In this study, a specific, accurate, linear, precise, and repeatable method was optimized, verified, and applied for the simultaneous estimation of artesunate and amodiaquine HCl in a commercially available artesunate-amodiaquine tablet with a dosage of 100 mg/270 mg. The optimization process involved two steps. Firstly, the top three were carefully selected out of seven characteristics influencing the separation. These key elements required fine-tuning, namely the column type, ion pair, and the residual amount of acetonitrile (ACN) remaining after elution. In the second step, a Box-Behnken experimental design, coupled with Derrenguer's desirability approach, was utilized to identify the ideal target conditions. The optimized method demonstrated excellent specificity, accuracy, linearity, precision, and repeatability, allowing for the reliable simultaneous estimation of artesunate and amodiaquine HCl in the artesunate-amodiaquine tablet. This method offers a valuable tool for quality control and dosage determination in the pharmaceutical industry. By employing advanced experimental techniques and focusing on critical parameters, the study contributes to analytical methodologies in malaria treatment.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"1 1","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67436967","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Study of the Biochemical Potential of Wild Fruit of the Caucasus Medar (Mespilus caucasics L.) in the Post-Harvest Period","authors":"É. B. Farzaliev","doi":"10.17721/moca.2023.29-32","DOIUrl":"https://doi.org/10.17721/moca.2023.29-32","url":null,"abstract":"The carbohydrate complex (fructose, glucose, sucrose, pectin substances), the main organic and fatty acids, which are important food functional ingredients, were studied in the wild fruits of the Caucasian loquat during their storage. It has been established that during 40 days of storage there are significant changes in the biochemical potential of fruits for almost all the studied food ingredients, the level of their final content is 5-10 % of the original content.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"1 1","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67436870","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Application of Enzymatic Photometric Kinetic Method for Determination of Benzalkonium Chloride in Various Dosage Forms","authors":"M. Blazheyevskіy, O. Koval’ska","doi":"10.17721/moca.2023.5-12","DOIUrl":"https://doi.org/10.17721/moca.2023.5-12","url":null,"abstract":"A kinetic-photometric method for accurate and sensitive determination of benzalconium chloride has been described. The method is based on inhibition of enzymatic hydrolysis of acetylcholine by enzyme acethylcholinestherase reaction. The amount of benzalconium chloride was determined by the degree of inhibition of the enzymatic reaction, which was evaluated by the residual unreacted substrate - acetylcholine. Determination of the residual amount of acetylcholine in the reaction mixture was performed by a kineticphotometric method using an indicator oxidation reaction of p-phenetidine with peracetic acid, which is formed during the auxiliration reaction of perhydrolysis with addition of excess hydrogen peroxide in the reaction mixture over a period of time. The inhibition degree –concentration plot is linear over the range of 1.4 ∙10-6 – 7.0∙10-6 mol/ L with correlation coefficient of 0.998. The LOQ was 1.9∙10-6 mol/L. The different experimental parameters pH, buffer solution was carefully studied and optimized. The proposed method has been successfully applied to pharmaceutical formulations. Statistical comparison of the results with a good established reported method showed excellent agreement and proved that there is no significant difference in the accuracy and precision. For “Virotec-intim” preparation RSD was 3.2 % (δ*=- 0.3 %).","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"1 1","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67437085","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Analytical Validation of a Reversed-Phase Ion Pairing HPLC-DAD Method for the Simultaneous Determination of Anthropogenic Pollutants","authors":"Liew Sook Ling, Ivan Kok Seng Yap, Chong Chun Wie, Wong Lai Chun","doi":"10.17721/moca.2023.13-21","DOIUrl":"https://doi.org/10.17721/moca.2023.13-21","url":null,"abstract":"Caffeine, trigonelline, nicotinamide, and hippuric acid are potential organic markers of anthropogenic activities in the environment. In this work, a selective, precise, accurate, and robust reverse phase high performance liquid chromatography with a diode array detection method was developed for their simultaneous determination. Chromatographic analysis was achieved on GraceSmart RP C18 (150 mm x 4.6 mm, 5 μm) column. The mobile phase was 20 mM ammonium acetate buffer (pH 4.5) and methanol in gradient elution mode at a flow rate of 1.0 mL min-1, with 5 mM heptafluorobutyric acid as an ion pairing agent. Detection was performed at 275 nm for caffeine, 265 nm for trigonelline, 261 nm for nicotinamide, and 250 nm for hippuric acid. The method was validated as per the International Conference on Harmonization guidelines. Linear responses were found in the concentration range of 10-200 μg mL-1 with a correlation coefficient of at least 0.999. The percent relative standard deviation of intra-day precision, inter-day precision, and robustness was less than 2 %. The accuracy, expressed as percentage recovery ranged between 93.23 – 99.22%. Values for limits of detection and quantification were between 0.07-0.34 μg mL-1, and 0.21-1.04 μg mL-1, respectively. Lake samples from public parks were collected and subjected to analysis using the validated method","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"1 1","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67437082","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Chromatographic Determination of the Chemical Composition of Apple Chips Extract","authors":"O. Hulai, V. Shemet, O.S. Klimovych","doi":"10.17721/moca.2023.33-41","DOIUrl":"https://doi.org/10.17721/moca.2023.33-41","url":null,"abstract":"The qualitative composition of the extraction of dried apples of green (Golden, Mutsu) and red (Florina, Aidared) varieties by gas-liquid chromatography with mass-selective detection has been established. The chips were obtained by convective drying at the temperature of +(63–70) °С to a final dampness of 6–8 %. Water-alcohol extract was analyzed on the Shimadzu GCMS-QP2020 gas chromatomas-spectrometer with a full ion current (SCAN), the scanning range of 40–1000 Da. The peaks were processed and identified based on the open source data (NIST 2017 and Wiley 5th Edition). In the studied samples of apple extraction, 30 characteristic components were found, among which carbohydrates predominate – mono- and disaccharides, their derivatives and products of dehydration and oxidation. The apple extract contains higher fatty acids: n-hexadecanoic acid, tetradecanoic acid, octadecanoic acid, oleic acid. Compounds formed as a result of drying (5-hydroxymethylfurfural, 3,5-dihydroxy-6-methyl-2,3-dihydro-4H-pyrane-4-one), as well as flavonoids and anthocyanins, which perform antioxidant and weak antibiotic functions in the body, were identified. Vitamins could not be determined using this method.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"1 1","pages":""},"PeriodicalIF":0.7,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67436937","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Simultaneous Quantitative Determination of Eight Fluoroquinolones by High-Performance Liquid Chromatography with UV Detection using a C18 Monolithic Column","authors":"Emna Toujani, Wafa Belgaied, Sana Toujani","doi":"10.17721/moca.2023.101-108","DOIUrl":"https://doi.org/10.17721/moca.2023.101-108","url":null,"abstract":"In the present work, an accurate and reliable reversed-phase liquid chromatographic method (RP-HPLC) for the simultaneous quantitative determination of eight fluoroquinolones (enoxacin, norfloxacin, ciprofloxacin, levofloxacin, moxifloxacin, enrofloxacin, sparfloxacin, and marbofloxacin) in bulk form and in pharmaceutical products is described. The optimum separation of the selected pharmaceutical compounds was achieved on a Chromolith® RP-18 endcapped column with a mobile phase consisting of acetonitrile and phosphate buffer (pH 5.5; 15 mM) pumped at 2 mL min-1. UV detection of all compounds was accomplished at 280 nm. The procedure was validated according to the International Conference on Harmonization (ICH) Q2 (R1) guideline. Good linear relationships were obtained (r ≥ 0.996) for all the analytes over their respective concentration ranges. Intra- and inter-day precision were less than 2 %. Recoveries were held in the range of 98 to 102 %. The developed method was successfully applied to the analysis of pharmaceutical products.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"35 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135401568","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Partial Least Squares Method for the Multicomponent Analysis of Antibacterial Mixture","authors":"Farah Nouri, Nahla A. Alassaf","doi":"10.17721/moca.2023.92-100","DOIUrl":"https://doi.org/10.17721/moca.2023.92-100","url":null,"abstract":"This study's objective is to assess how well UV spectrophotometry can be used in conjunction with multivariate calibration based on partial least squares (PLS) regression for concurrent quantitative analysis of antibacterial mixture (Levofloxacin (LIV), Metronidazole (MET), Rifampicin (RIF) and Sulfamethoxazole (SUL)) in their artificial mixtures and pharmaceutical formulations. The experimental calibration and validation matrixes were created using 42 and 39 samples, respectively. The concentration range taken into account was 0-17 μg/mL for all components. The calibration standards' absorbance measurements were made between 210 and 350 nm, with intervals of 0.2 nm. The associated parameters were examined in order to develop the optimal calibration model. The cross-validation method was used to determine the ideal number of components. The coefficient of determination (R2) and the root mean square error of calibration (RMSEC) are used to evaluate the calibration model. The relation between the LEV, MET, RIF, and SUL actual values and predicted values had a coefficient of determination that was higher than 0.997, showing very good accuracy of the devised approach. The obtained RMSEC values, 0.181056465 (LEV), 0.180375418 (MET), 0.142767171 (RIF), and 0.17157454 (SUL), show an analytical procedure with adequate precision. The suggested technique for quantitative analysis of the quaternary mixture of LEV, MET, RIF, and SUL have been applied successfully in different pharmaceutical preparations. The UV spectrophotometry assisted with chemometric-PLS without prior treatment, be utilised to resolve multicomponent mixtures successfully.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"171 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135401276","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Extraction of Alkaloids by the Micellar Phase of Sodium Dodecyl Sulfate for their Further Chromatographic Determination","authors":"V.S. Starova, S.A. Kulichenko","doi":"10.17721/moca.2023.81-86","DOIUrl":"https://doi.org/10.17721/moca.2023.81-86","url":null,"abstract":"The influence of the main parameters of hydrophobicity (log P), structure (PSA), and protolytic properties (pKa) of some alkaloids on their distribution into modified micellar extraction system based on sodium dodecyl sulfate (SDS-NaCl-H2Sal) was established. The proposed prognostic regression D= 941 – 4.09∙PSA – 27.3∙log P – 44.5∙рКа is characterized by satisfactory indexes (R-squared 99.9, F-ratio 242, standard error 7.19, mean absolute error 2.38). The accuracy of the alkaloid distribution prediction by this regression is well correlated with accuracy of the measurement of the extraction parameters. The predicted D value for novocaine is 257 (R = 93 %), and the experimentally found D value is 202 (R = 91 %). For lidocaine, the predicted and experimental D values are practically the same and equal 386 (R = 95 %) and 380 (R = 95 %), respectively. The possibility of quantitative extraction of positively charged hydrophilic (logP < 0) organic bases into the micellar phase of SDS is shown. The developed hybrid HPLC technique for determining papaverine in urine with its cationic form (pH=2) preconcentration by modified micellar SDS phase is characterized by sufficient sensitivity and accuracy (DL= 0.01 μg/ml, Sr ≤ 0.08, R > 99 %, K = 10). Only alkaloids with log P > 1.4 can be determined by this technique because otherwise, the chromatographic peaks of salicylic acid and alkaloid cannot separate.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":"86 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135402112","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}