Methods and Objects of Chemical Analysis最新文献

Development, Optimization, and Validation of a Novel HPLC Method for Simultaneous Quantification of Artesunate and Amodiaquine in Tablet Formulations 同时测定片剂中青蒿琥酯和阿莫地喹含量的高效液相色谱方法的建立、优化和验证

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Methods and Objects of Chemical Analysis Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.42-50

Fouad Echerfaoui, H. Bouchafra, K. El Bourakadi, A. El Orche, Mounir El Kacemi, Abdelhafid Benomar, K. Karrouchi, M. Bouatia, M. El Karbane

{"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":null,"pages":null},"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}

引用次数: 0

Study of the Biochemical Potential of Wild Fruit of the Caucasus Medar (Mespilus caucasics L.) in the Post-Harvest Period 高加索Medar (Mespilus caucasics L.)野生果实收获后生化势的研究

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Methods and Objects of Chemical Analysis Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.29-32

É. B. Farzaliev

引用次数: 0

Application of Enzymatic Photometric Kinetic Method for Determination of Benzalkonium Chloride in Various Dosage Forms 酶光度动力学法测定不同剂型苯扎氯铵的应用

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Methods and Objects of Chemical Analysis Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.5-12

M. Blazheyevskіy, O. Koval’ska

{"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":null,"pages":null},"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}

引用次数: 0

Analytical Validation of a Reversed-Phase Ion Pairing HPLC-DAD Method for the Simultaneous Determination of Anthropogenic Pollutants 反相离子配对HPLC-DAD法同时测定人为污染物的分析验证

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Methods and Objects of Chemical Analysis Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.13-21

Liew Sook Ling, Ivan Kok Seng Yap, Chong Chun Wie, Wong Lai Chun

{"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":null,"pages":null},"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}

引用次数: 0

Chromatographic Determination of the Chemical Composition of Apple Chips Extract 苹果片提取物化学成分的色谱测定

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Methods and Objects of Chemical Analysis Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.33-41

O. Hulai, V. Shemet, O.S. Klimovych

{"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":null,"pages":null},"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}

引用次数: 0

Simultaneous Quantitative Determination of Eight Fluoroquinolones by High-Performance Liquid Chromatography with UV Detection using a C18 Monolithic Column C18整体柱高效液相色谱-紫外检测同时定量测定8种氟喹诺酮类药物

Methods and Objects of Chemical Analysis Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.101-108

Emna Toujani, Wafa Belgaied, Sana Toujani

引用次数: 0

Partial Least Squares Method for the Multicomponent Analysis of Antibacterial Mixture 抗菌合剂多组分分析的偏最小二乘法

Methods and Objects of Chemical Analysis Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.92-100

Farah Nouri, Nahla A. Alassaf

{"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":null,"pages":null},"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}

引用次数: 0

Extraction of Alkaloids by the Micellar Phase of Sodium Dodecyl Sulfate for their Further Chromatographic Determination 十二烷基硫酸钠胶束相萃取生物碱的进一步色谱测定

Methods and Objects of Chemical Analysis Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.81-86

V.S. Starova, S.A. Kulichenko

{"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":null,"pages":null},"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}

引用次数: 0

Determination of Mycotoxins in Wheat Grain by LC-MS/MS using Modified QuEChERS Sample Preparation 改良QuEChERS样品制备的LC-MS/MS法测定小麦籽粒中的真菌毒素

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Methods and Objects of Chemical Analysis Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.22-28

S. Senin, S. Midyk, V. Korniyenko, O. Konovalova, O. V. Berezovskyi, E. Ladohubets, I. Harkusha

{"title":"Determination of Mycotoxins in Wheat Grain by LC-MS/MS using Modified QuEChERS Sample Preparation","authors":"S. Senin, S. Midyk, V. Korniyenko, O. Konovalova, O. V. Berezovskyi, E. Ladohubets, I. Harkusha","doi":"10.17721/moca.2023.22-28","DOIUrl":"https://doi.org/10.17721/moca.2023.22-28","url":null,"abstract":"The procedure of the mycotoxins determination in wheat grain was developed by LC-MS/MS using modified QuEChERS sample preparation. The method of simultaneous determination of six mycotoxins (aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, T-2 toxin and zearalenone) in wheat grain was validated according to the following criteria: specificity, linearity, limits of detection (LOD), limits of quantification (LOQ), accuracy, and precision. The chromatographic and mass spectrometric conditions for separation and determination of the mycotoxins were optimized during the study. It was established that the most optimal mobile phase for the separation of six mycotoxins is 5 mМ ammonium formate solution in methanol : water : formic acid (5 : 94.9 : 0.1 by volume, eluent A and 95:4.9:0.1 by volume, eluent B). It was found that the correlation coefficients for six mycotoxins range from 0.9990 to 0.9998 (R2 > 0.995). Limits of detection (LOD) and limits of quantification (LOQ) of the mycotoxins are below the maximum permitted levels set by the European Union (EU). Percent recovery in the range from 88 to 103 % indicates the acceptability of the mycotoxin extraction procedure. The relative standard deviation (RSD, %) of the measurement results under conditions of repeatability ranged from 1.94 to 8.76 %. The obtained data suitability evaluation of method (validation) corresponds to criteria European Commission Regulation (EC) No. 401/2006. The validation results showed that LC-MS/MS method with using of modified QuEChERS sample preparation is effective and suitable for the simultaneous quantitation of mycotoxins in wheat grain.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67437257","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}

引用次数: 0

Development of the Spectrophotometric Method for the Determination of Metoprolol in Tablets by using Bromothymol Blue 溴百里酚蓝分光光度法测定片剂中美托洛尔的含量

Methods and Objects of Chemical Analysis Pub Date : 2023-01-01 DOI: 10.17721/moca.2023.63-69

Mariana Horyn, Marjan Piponski, Oleksandra Melnyk, Iryna Ivanchuk, Oleksandr Susla, Liliia Grytsyshyn, Dmytro Korobko, Liliya Logoyda

{"title":"Development of the Spectrophotometric Method for the Determination of Metoprolol in Tablets by using Bromothymol Blue","authors":"Mariana Horyn, Marjan Piponski, Oleksandra Melnyk, Iryna Ivanchuk, Oleksandr Susla, Liliia Grytsyshyn, Dmytro Korobko, Liliya Logoyda","doi":"10.17721/moca.2023.63-69","DOIUrl":"https://doi.org/10.17721/moca.2023.63-69","url":null,"abstract":"A simple, eco-friendly, rapid, and economic spectrophotometric method for the determination of metoprolol tartrate in tablets has been developed. The procedure for metoprolol determination is based on a reaction with bromothymol blue (BTB) in acetonitrile medium. The maximum formation of the colored product was observed in acetonitrile at the absorption maximum at a wavelength of 402 nm. The stoichiometry of molecular complexes was determined by Job's method and it was found to be 1 to 1. The optimal concentration of BTB was 1.6·10-4 M. The linear relationship between absorbance at λmax and concentration of analyte ranging 16.00-24.00 μg mL-1 was found. Regression analysis of Beer’s law plot at 402 nm yielded the regression equation, y = 0.0199x + 0.0721. High values of correlations coefficient R2 = 0.9990 and small values of intercept validated the linearity of calibration curve and obedience to Beer’s law. The calculated LOD and LOQ values were 1.90 and 5.78 μg mL-1, respectively. The proposed green spectrophotometric method is simple, rapid, and suitable for routine pharmaceutical analysis.","PeriodicalId":18626,"journal":{"name":"Methods and Objects of Chemical Analysis","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135400866","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}

引用次数: 0