Pub Date : 2022-12-30DOI: 10.20450/mjcce.2022.2608
A. Milenković, J. Stanojević, L. Stanojević
The objective of this study was to analyze the chemical composition of the essential oil (EO) and hydrolate of black pepper fruit, as well as their antioxidant activity. The EO was obtained by Clevenger-type hydrodistillation with hydromodule 1:10 m/v for 240 minutes, and the hydrolate was collected after the hydrodistillation process. The qualitative composition of EO was determined by GC/MS and quantitative by GC/FID method, while the qualitative composition of a hydrolate was determined by HS-SPME-GC/MS and quantitative composition by HS-SPME-GC/FID method. The antioxidant activity was investigated by DPPH assay. Fifty-five compounds were identified from black pepper EO, where the most abundant compounds were (E)-caryophyllene (41.6 %), limonene (9.7 %), and sabinene (8.6 %). Twelve compounds were identified from black pepper hydrolate, where the most abundant compounds were α-terpineol (34.7 %), borneol (17.3 %), and terpinen-4-ol (13.9 %). The hydrolate showed higher antioxidant activity after 20 minutes of incubation with an EC50 value of 0.993 ± 0.011 mg/cm3 compared to the EO with an EC50 value of 67.72 ± 1.871 mg/cm3. According to the results obtained in this study, both the EO and hydrolate are good sources of natural antioxidants with potential uses in the food, organic agriculture, pharmaceutical, and cosmetic industries as a safer alternative to synthetic additives. Furthermore, the possibility of wider uses of the hydrolate should be investigated in more detail. Although researchers interested in hydrolate investigation focus mostly on their antioxidant activity, these "aromatic wastes" could also present promising cosmetic activities.
{"title":"Comparative analysis of chemical composition and antioxidant activity of essential oil and hydrolate from black pepper fruit (Piper nigrum L.)","authors":"A. Milenković, J. Stanojević, L. Stanojević","doi":"10.20450/mjcce.2022.2608","DOIUrl":"https://doi.org/10.20450/mjcce.2022.2608","url":null,"abstract":"The objective of this study was to analyze the chemical composition of the essential oil (EO) and hydrolate of black pepper fruit, as well as their antioxidant activity. The EO was obtained by Clevenger-type hydrodistillation with hydromodule 1:10 m/v for 240 minutes, and the hydrolate was collected after the hydrodistillation process. The qualitative composition of EO was determined by GC/MS and quantitative by GC/FID method, while the qualitative composition of a hydrolate was determined by HS-SPME-GC/MS and quantitative composition by HS-SPME-GC/FID method. The antioxidant activity was investigated by DPPH assay. Fifty-five compounds were identified from black pepper EO, where the most abundant compounds were (E)-caryophyllene (41.6 %), limonene (9.7 %), and sabinene (8.6 %). Twelve compounds were identified from black pepper hydrolate, where the most abundant compounds were α-terpineol (34.7 %), borneol (17.3 %), and terpinen-4-ol (13.9 %). The hydrolate showed higher antioxidant activity after 20 minutes of incubation with an EC50 value of 0.993 ± 0.011 mg/cm3 compared to the EO with an EC50 value of 67.72 ± 1.871 mg/cm3.\u0000According to the results obtained in this study, both the EO and hydrolate are good sources of natural antioxidants with potential uses in the food, organic agriculture, pharmaceutical, and cosmetic industries as a safer alternative to synthetic additives. Furthermore, the possibility of wider uses of the hydrolate should be investigated in more detail. Although researchers interested in hydrolate investigation focus mostly on their antioxidant activity, these \"aromatic wastes\" could also present promising cosmetic activities.","PeriodicalId":18088,"journal":{"name":"Macedonian Journal of Chemistry and Chemical Engineering","volume":" ","pages":""},"PeriodicalIF":1.0,"publicationDate":"2022-12-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43030222","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}
Pub Date : 2022-06-30DOI: 10.20450/mjcce.2022.2404
R. Gulaboski, V. Mirčeski
Differential square-wave voltammetry (DSWV) is the most recent modification of square-wave voltammetry (SWV) developed for advancing the performances of the technique for both analytical and kinetics applications. The differential current-measuring protocol in DSWV leads to improved voltammetric features of the forward and backward current components, in particular when slow i.e., quasireversible or irreversible electrode reactions are studied. In the present theoretical work catalytic electrode mechanism of surface bounded redox species (surface EC’ mechanism) is studied under conditions of the new technique, where E denotes the electrode reaction and C’ refers to the irreversible follow-up regenerative chemical reaction. Presented theoretical data provides a general overview of the EC’ reaction scheme, implying some specific voltammetric features which can be exploited for estimation of relevant physical parameters of the electrode reaction E and the regenerative chemical reaction C’.
{"title":"Surface catalytic mechanism-theoretical study under conditions of differential square-wave voltammetry","authors":"R. Gulaboski, V. Mirčeski","doi":"10.20450/mjcce.2022.2404","DOIUrl":"https://doi.org/10.20450/mjcce.2022.2404","url":null,"abstract":"Differential square-wave voltammetry (DSWV) is the most recent modification of square-wave voltammetry (SWV) developed for advancing the performances of the technique for both analytical and kinetics applications. The differential current-measuring protocol in DSWV leads to improved voltammetric features of the forward and backward current components, in particular when slow i.e., quasireversible or irreversible electrode reactions are studied. In the present theoretical work catalytic electrode mechanism of surface bounded redox species (surface EC’ mechanism) is studied under conditions of the new technique, where E denotes the electrode reaction and C’ refers to the irreversible follow-up regenerative chemical reaction. Presented theoretical data provides a general overview of the EC’ reaction scheme, implying some specific voltammetric features which can be exploited for estimation of relevant physical parameters of the electrode reaction E and the regenerative chemical reaction C’.","PeriodicalId":18088,"journal":{"name":"Macedonian Journal of Chemistry and Chemical Engineering","volume":" ","pages":""},"PeriodicalIF":1.0,"publicationDate":"2022-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45200551","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}
Pub Date : 2022-06-30DOI: 10.20450/mjcce.2022.2490
V. Petrushevski, K. Béres, P. Bombicz, A. Farkas, L. Kótai, L. Bereczki
Tetrapyridinesilver(I) perrhenate [Agpy4]ReO4 was synthesized, and its crystal structure and Raman spectra were elucidated at low temperatures. The crystal lattice is constructed from isolated tetrahedral cations and anions having no argentophilic interactions. Weak hydrogen bonds are formed between the oxygens of the disordered perrhenate anions and the ortho-hydrogens of the pyridine ligands. No parallel π…π stacking interactions are observed, but C-H…π interactions of the pyridine ligands within columns of cations and between the columns appeared. Correlation analysis for Ag+, pyridine ligands, and perrhenate ions was performed, and the perrhenate ion and some of the AgN4 skeleton vibrational modes and pyridine ligand modes in the Raman spectrum of [Agpy4]ReO4 were assigned.
{"title":"Structural and Raman spectroscopic characterization of tetrapyridinesilver(I) perrhenate, [Agpy4]ReO4","authors":"V. Petrushevski, K. Béres, P. Bombicz, A. Farkas, L. Kótai, L. Bereczki","doi":"10.20450/mjcce.2022.2490","DOIUrl":"https://doi.org/10.20450/mjcce.2022.2490","url":null,"abstract":"Tetrapyridinesilver(I) perrhenate [Agpy4]ReO4 was synthesized, and its crystal structure and Raman spectra were elucidated at low temperatures. The crystal lattice is constructed from isolated tetrahedral cations and anions having no argentophilic interactions. Weak hydrogen bonds are formed between the oxygens of the disordered perrhenate anions and the ortho-hydrogens of the pyridine ligands. No parallel π…π stacking interactions are observed, but C-H…π interactions of the pyridine ligands within columns of cations and between the columns appeared. Correlation analysis for Ag+, pyridine ligands, and perrhenate ions was performed, and the perrhenate ion and some of the AgN4 skeleton vibrational modes and pyridine ligand modes in the Raman spectrum of [Agpy4]ReO4 were assigned.","PeriodicalId":18088,"journal":{"name":"Macedonian Journal of Chemistry and Chemical Engineering","volume":" ","pages":""},"PeriodicalIF":1.0,"publicationDate":"2022-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41909051","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}
Pub Date : 2022-06-30DOI: 10.20450/mjcce.2022.2403
S. Kawsar, M. Ouassaf, Samir CHTITA, Aishi Barua Jui, S. Belaidi
Currently, methyl-β-D-galactopyranoside (MDG) esters have become a focus of attention due to their promising biological and pharmacokinetic properties and could be a good choice in unraveling the global issue of pathogenic multidrug resistance. Structural modification of MDG can improve its mode of biological activity. In line with these efforts, a series of previously synthesized MDG esters were designed and evaluated by Prediction of Activity Spectra for Substances (PASS), molecular docking simulation, and pharmacokinetic depiction. Encouraging PASS activity was observed for several aliphatic and aromatic MDG esters, and antibacterial efficacy was more promising than other features. In support, molecular docking studies were performed against the macrolide phosphotransferase enzyme MPH to identify a potential allosteric binding site for these esters. Molecular docking indicated that the shape of the MDG esters and their ability to form multiple electrostatic and hydrogen bonds with the active site corresponds to the binding modes of other minor-groove binders. Pharmacokinetic predictions were also performed to evaluate the absorption, metabolism, and toxic properties of MDG esters. These findings demonstrate that MDG esters are promising for use as biocompatible antibacterial agents in the future.
{"title":"PASS prediction, molecular docking and pharmacokinetic studies of acyl substituted bioactive galactopyranoside esters as antibacterial agents","authors":"S. Kawsar, M. Ouassaf, Samir CHTITA, Aishi Barua Jui, S. Belaidi","doi":"10.20450/mjcce.2022.2403","DOIUrl":"https://doi.org/10.20450/mjcce.2022.2403","url":null,"abstract":"Currently, methyl-β-D-galactopyranoside (MDG) esters have become a focus of attention due to their promising biological and pharmacokinetic properties and could be a good choice in unraveling the global issue of pathogenic multidrug resistance. Structural modification of MDG can improve its mode of biological activity. In line with these efforts, a series of previously synthesized MDG esters were designed and evaluated by Prediction of Activity Spectra for Substances (PASS), molecular docking simulation, and pharmacokinetic depiction. Encouraging PASS activity was observed for several aliphatic and aromatic MDG esters, and antibacterial efficacy was more promising than other features. In support, molecular docking studies were performed against the macrolide phosphotransferase enzyme MPH to identify a potential allosteric binding site for these esters. Molecular docking indicated that the shape of the MDG esters and their ability to form multiple electrostatic and hydrogen bonds with the active site corresponds to the binding modes of other minor-groove binders. Pharmacokinetic predictions were also performed to evaluate the absorption, metabolism, and toxic properties of MDG esters. These findings demonstrate that MDG esters are promising for use as biocompatible antibacterial agents in the future.","PeriodicalId":18088,"journal":{"name":"Macedonian Journal of Chemistry and Chemical Engineering","volume":" ","pages":""},"PeriodicalIF":1.0,"publicationDate":"2022-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43194676","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}
Pub Date : 2022-06-30DOI: 10.20450/mjcce.2022.2381
Öznur Güngör
In this study, an electrochemical sensor based on a boron doped diamond electrode (BDDE) was developed for the determination of naproxen (NAP) using a poly(aniline-2-sulfonic acid)/boron doped diamond electrode, p(A2SA/BDDE). Polymerization of A2SA was conducted in a water/acetonitrile (1:1) mixture containing 0.1 M sodium perchlorate (NaClO4) on bare BDDE and the electrochemical properties studied by cyclic voltammetry in ferricyanide/KNO3 solution. The prepared p(A2SA/BDDE) was used for detection of NAP. Effects of parameters such as monomer type and concentration, the number of cycles, and scan rate were investigated using differential pulse voltammetry (DPV) in phosphate buffer containing 0.75 mM NAP. The effect of electrolyte type and pH on DPV responses to NAP were also studied. The oxidative current peak stem from NAP concentration observed at 1.1 V potential. A linear calibration curve was obtained in the range of 0.05–1.00 mM NAP concentration. Correlation coefficient (R2), detection limit, and quantification limit were calculated as 0.9944, 0.0328 mM, and 0.1093 mM, respectively. In conclusion, it may be claimed that the modified electrode constructed in this work can be used successfully as a naproxen-selective membrane due to its ease of preparation, high R2 value, and good reproducibility.
本研究采用聚苯胺-2-磺酸/硼掺杂金刚石电极p(A2SA/BDDE)，建立了一种基于硼掺杂金刚石电极(BDDE)的电化学传感器，用于萘普生(NAP)的测定。在含有0.1 M高氯酸钠(NaClO4)的水/乙腈(1:1)混合物中对裸BDDE进行了A2SA的聚合，并在铁氰化物/KNO3溶液中采用循环伏安法研究了A2SA的电化学性能。制备的p(A2SA/BDDE)用于检测NAP。在含0.75 mM NAP的磷酸盐缓冲液中，采用差分脉冲伏安法(DPV)研究了单体类型、浓度、循环次数、扫描速率等参数对磷酸基磷酸酯的影响。研究了电解质类型和pH对DPV对NAP反应的影响。氧化电流峰值来源于在1.1 V电位下观察到的NAP浓度。在0.05 ~ 1.00 mM NAP浓度范围内，得到线性校准曲线。相关系数(R2)为0.9944 mM，检出限为0.0328 mM，定量限为0.1093 mM。综上所述，本研究构建的修饰电极制备简单、R2值高、重现性好，可以成功地作为萘普生选择性膜。
{"title":"Determination of naproxen by using differential pulse voltammetry with poly (aniline-2-sulfonic acid) modified boron doped diamond electrode","authors":"Öznur Güngör","doi":"10.20450/mjcce.2022.2381","DOIUrl":"https://doi.org/10.20450/mjcce.2022.2381","url":null,"abstract":"In this study, an electrochemical sensor based on a boron doped diamond electrode (BDDE) was developed for the determination of naproxen (NAP) using a poly(aniline-2-sulfonic acid)/boron doped diamond electrode, p(A2SA/BDDE). Polymerization of A2SA was conducted in a water/acetonitrile (1:1) mixture containing 0.1 M sodium perchlorate (NaClO4) on bare BDDE and the electrochemical properties studied by cyclic voltammetry in ferricyanide/KNO3 solution. The prepared p(A2SA/BDDE) was used for detection of NAP. Effects of parameters such as monomer type and concentration, the number of cycles, and scan rate were investigated using differential pulse voltammetry (DPV) in phosphate buffer containing 0.75 mM NAP. The effect of electrolyte type and pH on DPV responses to NAP were also studied. The oxidative current peak stem from NAP concentration observed at 1.1 V potential. A linear calibration curve was obtained in the range of 0.05–1.00 mM NAP concentration. Correlation coefficient (R2), detection limit, and quantification limit were calculated as 0.9944, 0.0328 mM, and 0.1093 mM, respectively. In conclusion, it may be claimed that the modified electrode constructed in this work can be used successfully as a naproxen-selective membrane due to its ease of preparation, high R2 value, and good reproducibility.","PeriodicalId":18088,"journal":{"name":"Macedonian Journal of Chemistry and Chemical Engineering","volume":" ","pages":""},"PeriodicalIF":1.0,"publicationDate":"2022-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42865015","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}
Pub Date : 2022-06-30DOI: 10.20450/mjcce.2022.2493
Cemre Zeynep Harman, Öznur Güngör
A novel electrochemical sensor for testosterone detection has been prepared by the chemical modification of a gold electrode (AuE). For the electrode modification, specific polyurethane (PU) films were synthesized from hexamethylene diisocyanate, olivetol, polyethylene glycol-100 (PEG100) and β-cyclodextrin. The synthesized PUs were investigated as selective films, and were used to coat a AuE surface at different concentrations and thicknesses. The testosterone responses of the modified electrodes were investigated by square-wave voltammetry (SWV). One separated cathodic SWV peak was obtained for testosterone at –0.390 V, with the prepared PU-modified AuE in 0.1 M phosphate buffer (PB) (pH 7.2). The linearity of testosterone responses of the prepared PU modified electrode was obtained over a concentration range of 0.1–1.0 µM (R2 = 0.995). It was observed that the response of the electrode increased regularly and sensitively with increasing testosterone amount. The detection limit, relative standard deviation and sensitivity of modified electrode were found to be approximately 5.69 nM, 1.669 % and 98.331 %, respectively. The PU-modified AuE exhibited good selectivity and a low response time for testosterone. Therefore, the prepared testosterone sensor offers a good alternative for fast and practical testosterone determination in clinical or biomedical studies.
{"title":"Preparation of a polyurethane membrane testosterone sensor and its application using square-wave stripping voltammetry","authors":"Cemre Zeynep Harman, Öznur Güngör","doi":"10.20450/mjcce.2022.2493","DOIUrl":"https://doi.org/10.20450/mjcce.2022.2493","url":null,"abstract":"A novel electrochemical sensor for testosterone detection has been prepared by the chemical modification of a gold electrode (AuE). For the electrode modification, specific polyurethane (PU) films were synthesized from hexamethylene diisocyanate, olivetol, polyethylene glycol-100 (PEG100) and β-cyclodextrin. The synthesized PUs were investigated as selective films, and were used to coat a AuE surface at different concentrations and thicknesses. The testosterone responses of the modified electrodes were investigated by square-wave voltammetry (SWV). One separated cathodic SWV peak was obtained for testosterone at –0.390 V, with the prepared PU-modified AuE in 0.1 M phosphate buffer (PB) (pH 7.2). The linearity of testosterone responses of the prepared PU modified electrode was obtained over a concentration range of 0.1–1.0 µM (R2 = 0.995). It was observed that the response of the electrode increased regularly and sensitively with increasing testosterone amount. The detection limit, relative standard deviation and sensitivity of modified electrode were found to be approximately 5.69 nM, 1.669 % and 98.331 %, respectively. The PU-modified AuE exhibited good selectivity and a low response time for testosterone. Therefore, the prepared testosterone sensor offers a good alternative for fast and practical testosterone determination in clinical or biomedical studies.","PeriodicalId":18088,"journal":{"name":"Macedonian Journal of Chemistry and Chemical Engineering","volume":" ","pages":""},"PeriodicalIF":1.0,"publicationDate":"2022-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44939496","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}
Pub Date : 2022-06-30DOI: 10.20450/mjcce.2022.2478
Elena Trajchova Kovachovska, J. Acevska, K. Brezovska, Stefan Trajkovic, Ivana Mitrevska, S. Ugarkovic, A. Dimitrovska
This research highlights the specificity of the new stability-indicating method developed to evaluate the impurity profile of Atorvastatin film-coated tablets. The proposed method has the ability to capture any possible changes that may occur during the stability studies over time and under different stress factors, and is selective enough to enable quality control of finished product from different suppliers of active pharmaceutical ingredient (API)/excipients. Satisfactory critical peak resolution between specified and unspecified impurities was achieved using the fused-core shell technology and extensively endcapped diisopropyl-cyanopropylsilane stationary phase (Halo ES-CN 150 mm × 4.6 mm, 2.7 µm), with a 10 mM ammonium formate buffer pH 3.5 and acetonitrile as mobile phase. A potential worse case impurity profile was assumed by using retained samples combined with the data obtained for samples manufactured with APIs from different suppliers exposed to the forced degradation study. The mass balance for stressed samples demonstrated the stability-indicating capability of the proposed method.
{"title":"Development of a stability-indicating method for evaluation of impurity profile of Atorvastatin film-coated tablets using cyano column based on core-shell technology","authors":"Elena Trajchova Kovachovska, J. Acevska, K. Brezovska, Stefan Trajkovic, Ivana Mitrevska, S. Ugarkovic, A. Dimitrovska","doi":"10.20450/mjcce.2022.2478","DOIUrl":"https://doi.org/10.20450/mjcce.2022.2478","url":null,"abstract":"This research highlights the specificity of the new stability-indicating method developed to evaluate the impurity profile of Atorvastatin film-coated tablets. The proposed method has the ability to capture any possible changes that may occur during the stability studies over time and under different stress factors, and is selective enough to enable quality control of finished product from different suppliers of active pharmaceutical ingredient (API)/excipients. \u0000Satisfactory critical peak resolution between specified and unspecified impurities was achieved using the fused-core shell technology and extensively endcapped diisopropyl-cyanopropylsilane stationary phase (Halo ES-CN 150 mm × 4.6 mm, 2.7 µm), with a 10 mM ammonium formate buffer pH 3.5 and acetonitrile as mobile phase. A potential worse case impurity profile was assumed by using retained samples combined with the data obtained for samples manufactured with APIs from different suppliers exposed to the forced degradation study. The mass balance for stressed samples demonstrated the stability-indicating capability of the proposed method.","PeriodicalId":18088,"journal":{"name":"Macedonian Journal of Chemistry and Chemical Engineering","volume":"1 1","pages":""},"PeriodicalIF":1.0,"publicationDate":"2022-06-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41618748","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}
Pub Date : 2022-06-22DOI: 10.20450/mjcce.2022.2422
B. Stojanovska Dimzoska, Zehra Hajrulai Musliu, Risto Uzunov, A. Angeleska, K. Blagoevska, Radmila Crceva Nikolovska, G. Ilievska, Elizabeta Dimitrieska Stojkovic
A different, reliable, and cost-effective strategy for the analysis of aflatoxins, ochratoxin A, and zearalenone in corn-based foods was proposed, including one multi-toxin immunoaffinity column (IAC) sample preparation and three different high-performance liquid chromatography fluorescence detection methods. The analytical procedures were tested and verified, keeping in mind their occurrence at trace levels in corn-based foods. With the validation of the proposed multi-toxin IAC methodology and comparison of the performance characteristics with methods using a single-toxin IAC, we confirmed the reliability of the multi-toxin IAC procedure versus the single-toxin IAC. The methods were validated by revealing satisfactory performance characteristics; for example, the obtained values of limit of detection were significantly lower than the maximum limits for all mycotoxins of concern. In addition, the recovery values were between 70.9 % and 106.1 % for all mycotoxins of interest, with precision values lower than 10.5 %.
{"title":"Application of reliable cost-effective strategy for analysis of mycotoxins in corn-based foods with HPLC-FLD after multi-toxin immunoaffinity clean-up","authors":"B. Stojanovska Dimzoska, Zehra Hajrulai Musliu, Risto Uzunov, A. Angeleska, K. Blagoevska, Radmila Crceva Nikolovska, G. Ilievska, Elizabeta Dimitrieska Stojkovic","doi":"10.20450/mjcce.2022.2422","DOIUrl":"https://doi.org/10.20450/mjcce.2022.2422","url":null,"abstract":"A different, reliable, and cost-effective strategy for the analysis of aflatoxins, ochratoxin A, and zearalenone in corn-based foods was proposed, including one multi-toxin immunoaffinity column (IAC) sample preparation and three different high-performance liquid chromatography fluorescence detection methods. The analytical procedures were tested and verified, keeping in mind their occurrence at trace levels in corn-based foods. With the validation of the proposed multi-toxin IAC methodology and comparison of the performance characteristics with methods using a single-toxin IAC, we confirmed the reliability of the multi-toxin IAC procedure versus the single-toxin IAC. The methods were validated by revealing satisfactory performance characteristics; for example, the obtained values of limit of detection were significantly lower than the maximum limits for all mycotoxins of concern. In addition, the recovery values were between 70.9 % and 106.1 % for all mycotoxins of interest, with precision values lower than 10.5 %.\u0000 ","PeriodicalId":18088,"journal":{"name":"Macedonian Journal of Chemistry and Chemical Engineering","volume":" ","pages":""},"PeriodicalIF":1.0,"publicationDate":"2022-06-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43387257","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}
Pub Date : 2022-06-21DOI: 10.20450/mjcce.2022.2518
M. Najdoski, Z. Zdravkovski
A unique collection of samples of the chemical elements has been created and displayed at our Institute of Chemistry. Although whole collections are now commercially available, we decided to use, as much as possible, samples from local resources. The general idea was for each item to have a story, making it more interesting for the students and visitors. We were able to acquire elemental samples mined in Macedonia. Other samples were from our student and research labs, as well as donations from colleagues, and the rest were obtained from commercial sources. A web page was created with all the information on each sample, some of them containing videos. Next to the noble gases, mini Tesla coils were mounted to light up the gases.
{"title":"Elementary, my dear Watson! The making of a collection of the natural elements","authors":"M. Najdoski, Z. Zdravkovski","doi":"10.20450/mjcce.2022.2518","DOIUrl":"https://doi.org/10.20450/mjcce.2022.2518","url":null,"abstract":"A unique collection of samples of the chemical elements has been created and displayed at our Institute of Chemistry. Although whole collections are now commercially available, we decided to use, as much as possible, samples from local resources. The general idea was for each item to have a story, making it more interesting for the students and visitors. We were able to acquire elemental samples mined in Macedonia. Other samples were from our student and research labs, as well as donations from colleagues, and the rest were obtained from commercial sources. A web page was created with all the information on each sample, some of them containing videos. Next to the noble gases, mini Tesla coils were mounted to light up the gases.","PeriodicalId":18088,"journal":{"name":"Macedonian Journal of Chemistry and Chemical Engineering","volume":" ","pages":""},"PeriodicalIF":1.0,"publicationDate":"2022-06-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41656385","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}
Pub Date : 2022-06-21DOI: 10.20450/mjcce.2022.2483
V. Ivanova, A. Trendafilova
A closed-vessel microwave-assisted extraction (MAE) of phenolic compounds from the aerial parts of Inula britannica L. using single-factor experiments and the Box-Behnken design with four independent variables (liquid-to-solid ratio, ethanol concentration, extraction time, and temperature) was investigated. The ANOVA results showed that the obtained model was significant at a 95 % confidence level. The extraction parameters for the maximal total phenolic content (46.19 mg GAE/g DM) were determined to be 15.13 ml/g liquid-to-solid ratio, 55.95 % EtOH, 73.74 ºC, and 5.73 min. Compared with classical maceration, the proposed MAE of phenolic compounds from I. britannica saves a lot of time and gives a high extraction yield.
{"title":"Optimization of microwave-assisted extraction of phenolic compounds from Inula britannica L. using the Box-Behnken design","authors":"V. Ivanova, A. Trendafilova","doi":"10.20450/mjcce.2022.2483","DOIUrl":"https://doi.org/10.20450/mjcce.2022.2483","url":null,"abstract":"A closed-vessel microwave-assisted extraction (MAE) of phenolic compounds from the aerial parts of Inula britannica L. using single-factor experiments and the Box-Behnken design with four independent variables (liquid-to-solid ratio, ethanol concentration, extraction time, and temperature) was investigated. The ANOVA results showed that the obtained model was significant at a 95 % confidence level. The extraction parameters for the maximal total phenolic content (46.19 mg GAE/g DM) were determined to be 15.13 ml/g liquid-to-solid ratio, 55.95 % EtOH, 73.74 ºC, and 5.73 min. Compared with classical maceration, the proposed MAE of phenolic compounds from I. britannica saves a lot of time and gives a high extraction yield.","PeriodicalId":18088,"journal":{"name":"Macedonian Journal of Chemistry and Chemical Engineering","volume":" ","pages":""},"PeriodicalIF":1.0,"publicationDate":"2022-06-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49630641","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}
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