Pub Date : 2021-08-18DOI: 10.25135/jcm.60.2105.2076
Irfan Capan, S. Servi, A. Aysal, Pshtiwan Raheem Sabır
Amygdalin, a cyanogenic glycoside mostly found in the bitter almond kernel, plays an important role in conventional and modern medicine applications. The high diastereomeric purity amygdalin was isolated with chromatographic purification methods and recrystallization. Amygdalin and neoamygdalin were separated chromatographically using the porous graphitic carbon column. Identification and confirmation of each molecule was performed with the ESI Quadrupole Time of Flight system coupled with a reversed phase LC.
{"title":"Isolation of amygdalin epimer at high diastereomeric purity and its structural characterization by spectroscopic and Q-TOF LC-MS methods","authors":"Irfan Capan, S. Servi, A. Aysal, Pshtiwan Raheem Sabır","doi":"10.25135/jcm.60.2105.2076","DOIUrl":"https://doi.org/10.25135/jcm.60.2105.2076","url":null,"abstract":"Amygdalin, a cyanogenic glycoside mostly found in the bitter almond kernel, plays an important role in conventional and modern medicine applications. The high diastereomeric purity amygdalin was isolated with chromatographic purification methods and recrystallization. Amygdalin and neoamygdalin were separated chromatographically using the porous graphitic carbon column. Identification and confirmation of each molecule was performed with the ESI Quadrupole Time of Flight system coupled with a reversed phase LC.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2021-08-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48189939","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}
Pub Date : 2020-12-01DOI: 10.25135/jcm.46.20.07.1734
D. Shah, Ishita I. Gondalia, V. Patel, Ashok Mahajan, U. Chhalotiya
: Accurate and precise reverse phase liquid chromatographic method has been developed for the estimation Remogliflozin etabonate in bulk and tablet dosage form. Reverse phase C18 column was used as stationary phase along with mixture of methanol:water (70:30%, v/v) as a mobile phase. Mobile phase flow rate was maintained at 1mL/min and analysis was performed at 229 nm. The method was linear in the concentration range of 1 – 25 μg/mL with correlation coefficient (r 2 ) 0.997. The proposed method was validated with respect to linearity, accuracy, precision and robustness as per ICH Q2 (R1) guideline. To find out the possible degradation pathway, forced degradation studies were performed. The degraded product peaks were well resolved from the pure drug peak with significant difference in their retention time value. The drug was found to be highly susceptible to acid and base hydrolysis. The developed method can be used for analysis of stability samples and routing quality control evaluation of Remogliflozin etabonate in
{"title":"Stability indicating liquid chromatographic method for the estimation of remogliflozin etabonate","authors":"D. Shah, Ishita I. Gondalia, V. Patel, Ashok Mahajan, U. Chhalotiya","doi":"10.25135/jcm.46.20.07.1734","DOIUrl":"https://doi.org/10.25135/jcm.46.20.07.1734","url":null,"abstract":": Accurate and precise reverse phase liquid chromatographic method has been developed for the estimation Remogliflozin etabonate in bulk and tablet dosage form. Reverse phase C18 column was used as stationary phase along with mixture of methanol:water (70:30%, v/v) as a mobile phase. Mobile phase flow rate was maintained at 1mL/min and analysis was performed at 229 nm. The method was linear in the concentration range of 1 – 25 μg/mL with correlation coefficient (r 2 ) 0.997. The proposed method was validated with respect to linearity, accuracy, precision and robustness as per ICH Q2 (R1) guideline. To find out the possible degradation pathway, forced degradation studies were performed. The degraded product peaks were well resolved from the pure drug peak with significant difference in their retention time value. The drug was found to be highly susceptible to acid and base hydrolysis. The developed method can be used for analysis of stability samples and routing quality control evaluation of Remogliflozin etabonate in","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2020-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42790714","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}
Pub Date : 2020-06-10DOI: 10.25135/jcm.40.20.04.1634
M. Kuloglu, T. Tekin, Zeynep Türkmen, Y. T. Demircan, S. Mercan
{"title":"Determination of doxylamine from a tea sample: A claim of drug facilitated crime","authors":"M. Kuloglu, T. Tekin, Zeynep Türkmen, Y. T. Demircan, S. Mercan","doi":"10.25135/jcm.40.20.04.1634","DOIUrl":"https://doi.org/10.25135/jcm.40.20.04.1634","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2020-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46556303","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}
Pub Date : 2020-06-10DOI: 10.25135/jcm.39.20.05.1653
Zeynep Turkmen
{"title":"Development of a densitometric HPTLC method for determination of 5-HMF in fruit-based baby foods in Turkey","authors":"Zeynep Turkmen","doi":"10.25135/jcm.39.20.05.1653","DOIUrl":"https://doi.org/10.25135/jcm.39.20.05.1653","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2020-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44233930","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}
Pub Date : 2020-06-10DOI: 10.25135/jcm.34.20.01.1524
E. Uysal, L. Liv, F. Fiçicioǧlu, M. Arifoviç
TUBITAK UME (National Metrology Institute of Turkey) Electrochemistry Laboratory established the primary level electrolytic conductivity measurement system in 2018. The objective of this work is to prove the accuracy of the established system with an acceptable uncertainty and to disseminate the traceability for electrolytic conductivity measurements. While the accuracy of the system was tested with the certified conductivity solutions, the accuracy of the software developed at TUBITAK UME was also tested. The cell constant was determined as 0.57986 cm at 25 °C by using certified conductivity solutions. The accuracy of the system was evaluated using the measurement of certified conductivity solutions and it was found that there was no significant difference between the results at 95% confidence level. Finally, “Evaluation of measurement data Guide to the expression of uncertainty in measurement” and “EA-4/02 M: 2013 Evaluation of the Uncertainty of Measurement in Calibration” guides were used to form the uncertainty budget for primary level electrolytic conductivity measurements.
{"title":"Primary level electrolytic conductivity measurements at National Metrology Institute of Turkey (TUBITAK UME)","authors":"E. Uysal, L. Liv, F. Fiçicioǧlu, M. Arifoviç","doi":"10.25135/jcm.34.20.01.1524","DOIUrl":"https://doi.org/10.25135/jcm.34.20.01.1524","url":null,"abstract":"TUBITAK UME (National Metrology Institute of Turkey) Electrochemistry Laboratory established the primary level electrolytic conductivity measurement system in 2018. The objective of this work is to prove the accuracy of the established system with an acceptable uncertainty and to disseminate the traceability for electrolytic conductivity measurements. While the accuracy of the system was tested with the certified conductivity solutions, the accuracy of the software developed at TUBITAK UME was also tested. The cell constant was determined as 0.57986 cm at 25 °C by using certified conductivity solutions. The accuracy of the system was evaluated using the measurement of certified conductivity solutions and it was found that there was no significant difference between the results at 95% confidence level. Finally, “Evaluation of measurement data Guide to the expression of uncertainty in measurement” and “EA-4/02 M: 2013 Evaluation of the Uncertainty of Measurement in Calibration” guides were used to form the uncertainty budget for primary level electrolytic conductivity measurements.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2020-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43165242","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}
Pub Date : 2020-06-10DOI: 10.25135/jcm.36.20.01.1532
Demet Di̇nçel, Hatice Olgan, Zeynep Canbaloğlu, S. Yalçin, A. Erkuçuk, Gizem Tırıs, A. Gören
Adulteration of dietary supplements are serious threats to public health in all around of world. Nowadays, in order to obtain the intended effect from natural remedies, the adulteration of natural products via artificial or harmful chemicals are increasing. A rapid LC-MS/MS method for determination of capsaicin and dihydrocapsaicin in dietary supplements via Fortis C18 (150 x 3 mm; 3 μm) column at 25 °C was developed and validated in a mixture of mobile phase A (1 % formic acid solution and 0.1 % ammonium formate in water) and B (1 % formic acid solution and 0.1 % ammonium formate in methanol) with gradient program at a flow rate of 0.35 mL/min. The recoveries of developed methods weytre obtained in the range of % 95.4-106.3 for capsaicin and % 96.3-108.9 for dihydrocapsaicin. This study shows that synthetic compound dihydrocapsaicin is widely use in dietary supplements products for adulteration to increase the effects of product without any declaration.
{"title":"Determination of dihydrocapsaicin adulteration in dietary supplements using LC-MS/MS","authors":"Demet Di̇nçel, Hatice Olgan, Zeynep Canbaloğlu, S. Yalçin, A. Erkuçuk, Gizem Tırıs, A. Gören","doi":"10.25135/jcm.36.20.01.1532","DOIUrl":"https://doi.org/10.25135/jcm.36.20.01.1532","url":null,"abstract":"Adulteration of dietary supplements are serious threats to public health in all around of world. Nowadays, in order to obtain the intended effect from natural remedies, the adulteration of natural products via artificial or harmful chemicals are increasing. A rapid LC-MS/MS method for determination of capsaicin and dihydrocapsaicin in dietary supplements via Fortis C18 (150 x 3 mm; 3 μm) column at 25 °C was developed and validated in a mixture of mobile phase A (1 % formic acid solution and 0.1 % ammonium formate in water) and B (1 % formic acid solution and 0.1 % ammonium formate in methanol) with gradient program at a flow rate of 0.35 mL/min. The recoveries of developed methods weytre obtained in the range of % 95.4-106.3 for capsaicin and % 96.3-108.9 for dihydrocapsaicin. This study shows that synthetic compound dihydrocapsaicin is widely use in dietary supplements products for adulteration to increase the effects of product without any declaration.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":"1 1","pages":""},"PeriodicalIF":1.3,"publicationDate":"2020-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41727560","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}
Pub Date : 2020-06-10DOI: 10.25135/jcm.33.20.04.1610
Züleyha Özer, S. Carikci, H. Yılmaz, T. Kilic, T. Dirmenci, A. Gören
{"title":"Determination of secondary metabolites of Origanum vulgare subsp. hirtum and O. vulgare subsp. vulgare by LC-MS/MS","authors":"Züleyha Özer, S. Carikci, H. Yılmaz, T. Kilic, T. Dirmenci, A. Gören","doi":"10.25135/jcm.33.20.04.1610","DOIUrl":"https://doi.org/10.25135/jcm.33.20.04.1610","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2020-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44941301","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}
Pub Date : 2020-06-10DOI: 10.25135/jcm.37.20.03.1583
A. Baysal, H. Saygin, G. Ustabasi
{"title":"Importance of sample pretreatment step on the bacterial toxicity bioassay of ZnO nanoparticles","authors":"A. Baysal, H. Saygin, G. Ustabasi","doi":"10.25135/jcm.37.20.03.1583","DOIUrl":"https://doi.org/10.25135/jcm.37.20.03.1583","url":null,"abstract":"","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2020-06-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48078421","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}
Pub Date : 2019-06-23DOI: 10.25135/JCM.25.19.04.1252
Eda Okuroglu, T. Tekin, M. Kuloglu, S. Mercan, I. Bavunoğlu, M. Acıkkol, Zeynep Türkmen
Caffeine is a substance that can be easily consumed in daily nutrition as well as in sport supplements. Exceeding the daily-recommended dose for caffeine may cause serious health problems. Studies illustrated that many concerns have been raising about the incompatibility between labels on sport supplements and their contents. The present study aimed to investigate caffeine contents in sport supplements purchased from Turkey market for the first time and to evaluate label information on products. Caffeine concentrations were determined in 41 sport supplements and possible adverse effects were emphasized considering calculated daily consumption doses. Seventeen samples among 41 products were found to be caffeine containing, ranging from 4.52 to 471 mg/mL. Three of caffeine containing products were undeclared their caffeine ingredients. Although three products were not specified caffeine their amounts, findings were found above the daily-recommended caffeine limit (400 mg/day). Significant differences were observed between the quantities indicated on the labels and the determined caffeine amounts in 7 products (p<0.05). Eight of 17 caffeine labelled products were found between 151-948% higher than stated label information. Overall, 29.4% of caffeine containing products (n=17) were found over the recommended intake. Consuming more than the daily-recommended dose may cause severe adverse reactions and consumers may experience serious health risks such as arterial hypertension, coronary heart disease, as well as sleep problems, irritability, anxiety, headache, and restlessness. Considering these health risks, awareness of consumers and accurate product labels on sport supplements gain more importance to prevent people from undesired consequences.
{"title":"Investigation of caffeine concentrations in sport supplements and inconsistencies in product labelling","authors":"Eda Okuroglu, T. Tekin, M. Kuloglu, S. Mercan, I. Bavunoğlu, M. Acıkkol, Zeynep Türkmen","doi":"10.25135/JCM.25.19.04.1252","DOIUrl":"https://doi.org/10.25135/JCM.25.19.04.1252","url":null,"abstract":"Caffeine is a substance that can be easily consumed in daily nutrition as well as in sport supplements. Exceeding the daily-recommended dose for caffeine may cause serious health problems. Studies illustrated that many concerns have been raising about the incompatibility between labels on sport supplements and their contents. The present study aimed to investigate caffeine contents in sport supplements purchased from Turkey market for the first time and to evaluate label information on products. Caffeine concentrations were determined in 41 sport supplements and possible adverse effects were emphasized considering calculated daily consumption doses. Seventeen samples among 41 products were found to be caffeine containing, ranging from 4.52 to 471 mg/mL. Three of caffeine containing products were undeclared their caffeine ingredients. Although three products were not specified caffeine their amounts, findings were found above the daily-recommended caffeine limit (400 mg/day). Significant differences were observed between the quantities indicated on the labels and the determined caffeine amounts in 7 products (p<0.05). Eight of 17 caffeine labelled products were found between 151-948% higher than stated label information. Overall, 29.4% of caffeine containing products (n=17) were found over the recommended intake. Consuming more than the daily-recommended dose may cause severe adverse reactions and consumers may experience serious health risks such as arterial hypertension, coronary heart disease, as well as sleep problems, irritability, anxiety, headache, and restlessness. Considering these health risks, awareness of consumers and accurate product labels on sport supplements gain more importance to prevent people from undesired consequences.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2019-06-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48751527","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}
Pub Date : 2019-06-23DOI: 10.25135/JCM.24.19.03.1219
H. Altundağ, E. Yıldırım, Esra Altintig
In this study, 20 fish taken from Sapanca Lake, Sakarya River and Western Black Sea (Karasu) in total and heavy metal accumulation (Cu, Fe abd Zn) in the muscles of 15 species was determined with ICP-OES (Inductively Coupled Plasma-Optical Emission Spectometer) device. When the results were examined, Cu, Fe and Zn concentration was determined to be 2.60-5.31 μg/g, 0.25-54.36 μg/g and 13.66-47.11 μg/g respectively in fish samples. In addition, the same procedures were applied with the standard reference material DORM-3 reference material (Fish Protein Certified Reference Material for Trace Metals) to determine the accuracy of the method. As a result, it has been determined that the amount of heavy metals contained in the analyzed fish samples is below the limit values provided by the Turkish Food Codex, Food and Agriculture Organization and World Health Organization and therefore consumption of these does not constitute a threat to health.
{"title":"Determination of some heavy metals by ICP-OES in edible parts of fish from Sapanca Lake and streams","authors":"H. Altundağ, E. Yıldırım, Esra Altintig","doi":"10.25135/JCM.24.19.03.1219","DOIUrl":"https://doi.org/10.25135/JCM.24.19.03.1219","url":null,"abstract":"In this study, 20 fish taken from Sapanca Lake, Sakarya River and Western Black Sea (Karasu) in total and heavy metal accumulation (Cu, Fe abd Zn) in the muscles of 15 species was determined with ICP-OES (Inductively Coupled Plasma-Optical Emission Spectometer) device. When the results were examined, Cu, Fe and Zn concentration was determined to be 2.60-5.31 μg/g, 0.25-54.36 μg/g and 13.66-47.11 μg/g respectively in fish samples. In addition, the same procedures were applied with the standard reference material DORM-3 reference material (Fish Protein Certified Reference Material for Trace Metals) to determine the accuracy of the method. As a result, it has been determined that the amount of heavy metals contained in the analyzed fish samples is below the limit values provided by the Turkish Food Codex, Food and Agriculture Organization and World Health Organization and therefore consumption of these does not constitute a threat to health.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":"1 1","pages":""},"PeriodicalIF":1.3,"publicationDate":"2019-06-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44563582","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}
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