Pub Date : 2023-03-10DOI: 10.25135/jcm.82.2301.2693
R. Kotadiya, Prachi Joshi
: Objectives: The ultraviolet spectrophotometric and reversed-phase high-performance liquid chromatography methods were developed and validated to quantify remogliflozin etabonate and vildagliptin in a fixed-dose tablet formulation. The materials and methods used in this study involved using methanol as the solvent in developing three ultraviolet spectrophotometric techniques, namely simultaneous equation, absorption ratio, and derivative spectroscopy. The wavelength maxima for vildagliptin and remogliflozin etabonate were determined to be 232 nm and 217 nm, respectively. The chromatographic method involved using a Phenomenex Luna C18 column (250 × 4.6 mm, 5 µm) and a mobile phase consisting of a mixture of methanol and acetate buffer (pH 5.6) in a 70:30 ratio. The flow rate was set at 1 mL/min, and the detecting wavelength was 210 nm. The results obtained from the optimized approaches met the performance test criteria set by the International Conference on Harmonization guideline Q2 (R1). The methods were then applied to assay marketed tablet formulations, and the results obtained were within acceptable limits. In conclusion, the developed techniques can be used to analyze the fixed-dose tablet formulation regularly.
：目的：建立并验证了紫外分光光度法和反相高效液相色谱法对固定剂量片剂中的依泊净和维达格利汀进行定量。本研究中使用的材料和方法包括以甲醇为溶剂开发三种紫外分光光度法，即联立方程、吸收比和导数光谱法。维达列汀和瑞格列嗪依他波酸的最大波长分别为232nm和217nm。色谱方法包括使用Phenomenex Luna C18柱（250×4.6 mm，5µm）和流动相，流动相由甲醇和乙酸缓冲液（pH 5.6）的混合物组成，比例为70:30。流速设定为1mL/min，检测波长为210nm。从优化方法中获得的结果符合国际协调会议准则Q2（R1）制定的性能测试标准。然后将这些方法应用于市场上销售的片剂配方的测定，得到的结果在可接受的限度内。总之，所开发的技术可以用于定期分析固定剂量片剂的配方。
{"title":"Simultaneous estimation of remogliflozin etabonate and vildagliptin in a tablet formulation: UV spectrophotometric and HPLC-PDA method","authors":"R. Kotadiya, Prachi Joshi","doi":"10.25135/jcm.82.2301.2693","DOIUrl":"https://doi.org/10.25135/jcm.82.2301.2693","url":null,"abstract":": Objectives: The ultraviolet spectrophotometric and reversed-phase high-performance liquid chromatography methods were developed and validated to quantify remogliflozin etabonate and vildagliptin in a fixed-dose tablet formulation. The materials and methods used in this study involved using methanol as the solvent in developing three ultraviolet spectrophotometric techniques, namely simultaneous equation, absorption ratio, and derivative spectroscopy. The wavelength maxima for vildagliptin and remogliflozin etabonate were determined to be 232 nm and 217 nm, respectively. The chromatographic method involved using a Phenomenex Luna C18 column (250 × 4.6 mm, 5 µm) and a mobile phase consisting of a mixture of methanol and acetate buffer (pH 5.6) in a 70:30 ratio. The flow rate was set at 1 mL/min, and the detecting wavelength was 210 nm. The results obtained from the optimized approaches met the performance test criteria set by the International Conference on Harmonization guideline Q2 (R1). The methods were then applied to assay marketed tablet formulations, and the results obtained were within acceptable limits. In conclusion, the developed techniques can be used to analyze the fixed-dose tablet formulation regularly.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2023-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48124890","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 : 2022-12-31DOI: 10.25135/jcm.80.2211.2667
S. Carikci, A. Gören, T. Kilic, T. Dirmenci
AbstrAbstract: Origanum majorana L., (OM), O. onites L. (OO) and O. syriacum L. (subsp. bevanii (Holmes) Greuter & Burdet) (OS) are belong to Majorana (Mill.) Benth. section of Origanum L. genus. In this study, quantities of some phenolic compounds; gallic acid, syringic acid, p -hydory benzoic acid, caffeic acid, ( E )-ferulic acid, chlorogenic acid, rosmarinic acid, pyrogallol and vanillin; in the chloroform (C), acetone (Ac) and methanol (M) extracts prepared from Origanum species collected from Türkiye were investigated via liquid chromatography and tandem mass spectrometry (LC-MS/MS). The relative standard deviations (RSD) of the phenolics were found as follows; 4.85, 8.39, 4.78, 8.04, 5.21, 5.45, 3.73, 5.47, respectively. Curcumin was used as an internal standard. In the extracts, ( E )-ferulic acid and caffeic acid were found to be the most abundant compounds. O. syriacum was determined as the richest species in terms of phenolic acids.
{"title":"Phenolic compounds from section Majorana (Mill.) Benth of Origanum L. species extracts via validated LC-MS/MS method","authors":"S. Carikci, A. Gören, T. Kilic, T. Dirmenci","doi":"10.25135/jcm.80.2211.2667","DOIUrl":"https://doi.org/10.25135/jcm.80.2211.2667","url":null,"abstract":"AbstrAbstract: Origanum majorana L., (OM), O. onites L. (OO) and O. syriacum L. (subsp. bevanii (Holmes) Greuter & Burdet) (OS) are belong to Majorana (Mill.) Benth. section of Origanum L. genus. In this study, quantities of some phenolic compounds; gallic acid, syringic acid, p -hydory benzoic acid, caffeic acid, ( E )-ferulic acid, chlorogenic acid, rosmarinic acid, pyrogallol and vanillin; in the chloroform (C), acetone (Ac) and methanol (M) extracts prepared from Origanum species collected from Türkiye were investigated via liquid chromatography and tandem mass spectrometry (LC-MS/MS). The relative standard deviations (RSD) of the phenolics were found as follows; 4.85, 8.39, 4.78, 8.04, 5.21, 5.45, 3.73, 5.47, respectively. Curcumin was used as an internal standard. In the extracts, ( E )-ferulic acid and caffeic acid were found to be the most abundant compounds. O. syriacum was determined as the richest species in terms of phenolic acids.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2022-12-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43849503","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 : 2022-12-31DOI: 10.25135/jcm.78.2211.2636
Mehul M. Patel, Komal Bansal
: In the present work, simple, precise, accurate high-performance thin-layer chromatography was developed, optimized, and validated for quantitation of Rivaroxaban (RIV) and Aspirin (ASP). The developed method was applied for quantification of both the drugs simultaneously in bulk drug and in-house tablet formulation. In this study, the Camag Linomat V HPTLC system and win CATS software V1.4.7 were used. Both molecules were separated using a chromatographic method consisting of toluene: ethyl acetate: methanol: glacial acetic acid (6:3:0.5:0.5 v/v/v/v) as mobile phase and an aluminum pre-coated plate with silica gel 60 F254 as the stationary phase. Both drugs were detected at 256nm. With R f values of 0.23 and 0.72, respectively, Rivaroxaban and Aspirin were satisfactorily resolved. Moreover, as per the ICHQ2 (R1) guideline, Specificity, precision, accuracy, robustness, linearity, the limit of detection, and the limit of quantification were performed. The method was found linear in the range of 100-400 ng/band and 2000-8000 ng/band of Rivaroxaban and Aspirin, respectively. The precision of the method was determined by %RSD and it was found in range. In-house tablet formulation was prepared and applied the developed method for assay of RIV and ASP. The % Assay (%v/v) of RIV and ASP was found 100.61 %w/w and 100.29 %w/w. In a conclusion, the accurate, precise, sensitive, and robust HPTLC method was optimized, developed, and validated as per ICH Q2 (R1) guideline, which was applied for in-house tablet formulation. The result of the assay suggests that the developed method can be used for simultaneous estimation of RIV and ASP for their dosage form as a part of regulatory submission.
：在本工作中，开发、优化并验证了简单、精确、准确的高效薄层色谱法用于定量利伐沙班（RIV）和阿司匹林（ASP）。所开发的方法用于同时定量散装药物和内部片剂中的两种药物。本研究使用Camag Linomat V HPTLC系统和win CATS软件V1.4.7。使用由甲苯：乙酸乙酯：甲醇：冰醋酸（6:3:0.5:0.5v/v/v）作为流动相和用硅胶60F254作为固定相的铝预涂板组成的色谱法分离两种分子。两种药物均在256nm处检测到。在Rf值分别为0.23和0.72的情况下，利伐沙班和阿司匹林得到了令人满意的解决。此外，根据ICHQ2（R1）指南，进行了特异性、精密度、准确性、稳健性、线性、检测限和定量限。该方法在利伐沙班和阿司匹林的100-400纳克/带和2000-8000纳克/带范围内分别呈线性。方法的精密度用%RSD测定，在范围内。制备了自制片剂，并应用所开发的RIV和ASP测定方法。RIV和ASP的%含量测定（%v/v）分别为100.61%w/w和100.29%w/w。总之，根据ICH Q2（R1）指南对准确、准确、灵敏和稳健的HPTLC方法进行了优化、开发和验证，该指南适用于内部片剂配方。测定结果表明，作为监管提交的一部分，所开发的方法可用于同时估计RIV和ASP的剂型。
{"title":"Development and application of HPTLC method for estimation of Rivaroxaban and Aspirin in bulk drug and in-house tablet form","authors":"Mehul M. Patel, Komal Bansal","doi":"10.25135/jcm.78.2211.2636","DOIUrl":"https://doi.org/10.25135/jcm.78.2211.2636","url":null,"abstract":": In the present work, simple, precise, accurate high-performance thin-layer chromatography was developed, optimized, and validated for quantitation of Rivaroxaban (RIV) and Aspirin (ASP). The developed method was applied for quantification of both the drugs simultaneously in bulk drug and in-house tablet formulation. In this study, the Camag Linomat V HPTLC system and win CATS software V1.4.7 were used. Both molecules were separated using a chromatographic method consisting of toluene: ethyl acetate: methanol: glacial acetic acid (6:3:0.5:0.5 v/v/v/v) as mobile phase and an aluminum pre-coated plate with silica gel 60 F254 as the stationary phase. Both drugs were detected at 256nm. With R f values of 0.23 and 0.72, respectively, Rivaroxaban and Aspirin were satisfactorily resolved. Moreover, as per the ICHQ2 (R1) guideline, Specificity, precision, accuracy, robustness, linearity, the limit of detection, and the limit of quantification were performed. The method was found linear in the range of 100-400 ng/band and 2000-8000 ng/band of Rivaroxaban and Aspirin, respectively. The precision of the method was determined by %RSD and it was found in range. In-house tablet formulation was prepared and applied the developed method for assay of RIV and ASP. The % Assay (%v/v) of RIV and ASP was found 100.61 %w/w and 100.29 %w/w. In a conclusion, the accurate, precise, sensitive, and robust HPTLC method was optimized, developed, and validated as per ICH Q2 (R1) guideline, which was applied for in-house tablet formulation. The result of the assay suggests that the developed method can be used for simultaneous estimation of RIV and ASP for their dosage form as a part of regulatory submission.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2022-12-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44220073","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 : 2022-12-31DOI: 10.25135/jcm.79.2211.2639
Andre Leesment, Sigrid Selberg, I. Leito
: NMR is a powerful technique with a wide range of applications, including measurements of acid dissociation constants (p K a values). One such example where NMR is particularly valuable is the measurement of biphasic octanol-water p K a (p K aow ) values. Acid-base properties in biphasic systems (extraction systems, lipid bilayers, phase-transfer catalysis systems) are commonly estimated from single-phase (typically aqueous) p K a values. However, acid-base properties in biphasic systems are more complex than in systems consisting of one phase and the single-phase p K a value does not adequately describe the situation. Biphasic p K a values (such as octanol:water biphasic p K a values, p K a ow ) have been introduced to provide a more realistic description of behaviour acids in biphasic systems. 1 H and 13 C NMR have been used extensively for p K a ow measurements and their advantages and disadvantages have been discussed in detail. However, the suitability of 31 P NMR has not yet been assessed in depth and 19 F NMR has until now not been used for p K a ow measurements at all. In this study, we measure p K a ow values with 1 H, 13 C, 19 F and 31 P NMR and provide a detailed comparison of NMR with these four nuclei in terms of p K aow measurement.
：核磁共振是一种强大的技术，具有广泛的应用，包括测量酸离解常数（p K a值）。NMR特别有价值的一个这样的例子是测量双相辛醇-水p K a（p K aow）值。双相系统（萃取系统、脂质双层、相转移催化系统）中的酸碱性质通常由单相（通常为水性）p K a值估计。然而，双相系统中的酸碱性质比单相系统中的更复杂，单相p K a值不能充分描述这种情况。引入了双相p K a值（如辛醇：水双相p K a值，p K a ow），以提供对双相系统中行为酸的更现实的描述。1H和13C NMR已被广泛用于p K a ow测量，并详细讨论了它们的优缺点。然而，31P NMR的适用性尚未得到深入评估，19F NMR迄今为止根本没有用于P K a ow测量。在这项研究中，我们用1H、13C、19F和31P NMR测量了pKaow值，并根据pKaow测量提供了NMR与这四个核的详细比较。
{"title":"NMR as biphasic pKa measurement technique","authors":"Andre Leesment, Sigrid Selberg, I. Leito","doi":"10.25135/jcm.79.2211.2639","DOIUrl":"https://doi.org/10.25135/jcm.79.2211.2639","url":null,"abstract":": NMR is a powerful technique with a wide range of applications, including measurements of acid dissociation constants (p K a values). One such example where NMR is particularly valuable is the measurement of biphasic octanol-water p K a (p K aow ) values. Acid-base properties in biphasic systems (extraction systems, lipid bilayers, phase-transfer catalysis systems) are commonly estimated from single-phase (typically aqueous) p K a values. However, acid-base properties in biphasic systems are more complex than in systems consisting of one phase and the single-phase p K a value does not adequately describe the situation. Biphasic p K a values (such as octanol:water biphasic p K a values, p K a ow ) have been introduced to provide a more realistic description of behaviour acids in biphasic systems. 1 H and 13 C NMR have been used extensively for p K a ow measurements and their advantages and disadvantages have been discussed in detail. However, the suitability of 31 P NMR has not yet been assessed in depth and 19 F NMR has until now not been used for p K a ow measurements at all. In this study, we measure p K a ow values with 1 H, 13 C, 19 F and 31 P NMR and provide a detailed comparison of NMR with these four nuclei in terms of p K aow measurement.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2022-12-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44219184","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 : 2022-12-17DOI: 10.25135/jcm.74.2209.2678
Celal Caner, Tuğba Özer, Esra Altintig, H. Altundağ
: In recent years, celiac disease has become known to the public with the development of medical diagnosis possibilities and increased awareness of the celiac disease. The only cure for celiac disease is a gluten-free diet that must be strictly followed for perpetuity. Food products with gluten content lower than 20 ppm are considered gluten-free products. With the increase in the number of people with celiac disease and people on a gluten-free diet, the amount and variety of gluten-free products have increased significantly. Rice and corn are the raw materials of gluten-free products. However, this situation causes people who follow a gluten-free diet to be exposed to a uniform diet and deficient in the intake of essential elements such as copper, iron, and manganese. In this study, 41 gluten-free products in Turkey were examined with ICP-OES as copper, iron, manganese, zinc, and strontium content, and the results were reported. The samples with the highest Cu concentration were corn and puffed rice at 51.45 mg/kg and vermicelli at 32.40 mg/kg. Chocolate sauce and cornflakes were the samples at 137.43 mg/kg and 117.20 mg/kg, respectively, with the highest Fe concentration. The highest Mn concentration was precooked chickpea flour at 20.80 mg/kg. The highest strontium concentration value was 12.85 mg/kg in carob flour. The samples with the highest Zn concentration were determined in yeast at 91.98 mg/kg and pistachio croquant at 85.50 mg/kg.
{"title":"Determination of some heavy metal deposits in gluten-free foods in Turkish market with ICP-OES","authors":"Celal Caner, Tuğba Özer, Esra Altintig, H. Altundağ","doi":"10.25135/jcm.74.2209.2678","DOIUrl":"https://doi.org/10.25135/jcm.74.2209.2678","url":null,"abstract":": In recent years, celiac disease has become known to the public with the development of medical diagnosis possibilities and increased awareness of the celiac disease. The only cure for celiac disease is a gluten-free diet that must be strictly followed for perpetuity. Food products with gluten content lower than 20 ppm are considered gluten-free products. With the increase in the number of people with celiac disease and people on a gluten-free diet, the amount and variety of gluten-free products have increased significantly. Rice and corn are the raw materials of gluten-free products. However, this situation causes people who follow a gluten-free diet to be exposed to a uniform diet and deficient in the intake of essential elements such as copper, iron, and manganese. In this study, 41 gluten-free products in Turkey were examined with ICP-OES as copper, iron, manganese, zinc, and strontium content, and the results were reported. The samples with the highest Cu concentration were corn and puffed rice at 51.45 mg/kg and vermicelli at 32.40 mg/kg. Chocolate sauce and cornflakes were the samples at 137.43 mg/kg and 117.20 mg/kg, respectively, with the highest Fe concentration. The highest Mn concentration was precooked chickpea flour at 20.80 mg/kg. The highest strontium concentration value was 12.85 mg/kg in carob flour. The samples with the highest Zn concentration were determined in yeast at 91.98 mg/kg and pistachio croquant at 85.50 mg/kg.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":"1 1","pages":""},"PeriodicalIF":1.3,"publicationDate":"2022-12-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41665235","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 : 2022-12-15DOI: 10.25135/jcm.752210.2596
Kul Aykut
: A simple and sensitive method has been developed for the simultaneous determination of chlorpheniramine maleate, pseudoephedrine hydrochloride, oxolamine citrate, and paracetamol by HPLC-PDA in pharmaceutical dosage forms. The separation of the analytes was achieved on an ACE 5 C8, 250 × 4.6 mm, 5 μm column using isocratic elution with a mobile phase containing methanol and 0.1 M phosphoric acid aqueous solution (15:85, v:v) at a flow rate of 1 mL/min. The total run time is 21 min. Chlorpheniramine maleate, pseudoephedrine hydrochloride, oxolamine citrate, and paracetamol were detected at wavelengths (retention times) of 264 nm (9.96 min), 205 nm (6.22 min), 239 nm (19.04 min) and 244 nm (5.22 min), respectively. The injection volume was 10 μL. The assay was in for chlorpheniramine maleate, pseudoephedrine hydrochloride, oxolamine citrate and paracetamol the concentration ranges 32–48 µg/mL, 9.6–14.4 µg/mL, 32–48 µg/mL, 104–156 µg/mL, respectively. LOQs (µg/mL) and LODs (µg/mL) 1.38 and 0.46 for chlorpheniramine maleate, 0.05 and 0.02 for pseudoephedrine hydrochloride, 0.76 and 0.25 for oxolamine citrate, 0.21 and 0.07 for paracetamol, respectively. Recoveries of the analytes were between 98% and 102% with intra-and inter-day precisions (as relative standard deviation) of ≤2%. In addition, expanded uncertainty values were less than 2 for all analytes. Method validation was carried out according to ICH guideline Q2 (R1). The analytical method validated was successfully applied to pharmaceutical dosage forms.
{"title":"Simultaneous determination of chlorpheniramine maleate, pseudoephedrine hydrochloride, oxolamine citrate and paracetamol by HPLC-PDA in pharmaceutical dosage forms","authors":"Kul Aykut","doi":"10.25135/jcm.752210.2596","DOIUrl":"https://doi.org/10.25135/jcm.752210.2596","url":null,"abstract":": A simple and sensitive method has been developed for the simultaneous determination of chlorpheniramine maleate, pseudoephedrine hydrochloride, oxolamine citrate, and paracetamol by HPLC-PDA in pharmaceutical dosage forms. The separation of the analytes was achieved on an ACE 5 C8, 250 × 4.6 mm, 5 μm column using isocratic elution with a mobile phase containing methanol and 0.1 M phosphoric acid aqueous solution (15:85, v:v) at a flow rate of 1 mL/min. The total run time is 21 min. Chlorpheniramine maleate, pseudoephedrine hydrochloride, oxolamine citrate, and paracetamol were detected at wavelengths (retention times) of 264 nm (9.96 min), 205 nm (6.22 min), 239 nm (19.04 min) and 244 nm (5.22 min), respectively. The injection volume was 10 μL. The assay was in for chlorpheniramine maleate, pseudoephedrine hydrochloride, oxolamine citrate and paracetamol the concentration ranges 32–48 µg/mL, 9.6–14.4 µg/mL, 32–48 µg/mL, 104–156 µg/mL, respectively. LOQs (µg/mL) and LODs (µg/mL) 1.38 and 0.46 for chlorpheniramine maleate, 0.05 and 0.02 for pseudoephedrine hydrochloride, 0.76 and 0.25 for oxolamine citrate, 0.21 and 0.07 for paracetamol, respectively. Recoveries of the analytes were between 98% and 102% with intra-and inter-day precisions (as relative standard deviation) of ≤2%. In addition, expanded uncertainty values were less than 2 for all analytes. Method validation was carried out according to ICH guideline Q2 (R1). The analytical method validated was successfully applied to pharmaceutical dosage forms.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2022-12-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45623761","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 : 2022-12-15DOI: 10.25135/jcm.76.2210.2601
D. Ozdemir, Dilek Tepeli, M. Gümüş
: In combination with a multivariate calibration method, FTIR-ATR spectroscopy was presented as a rapid method for the determination of some major oxides (CaO, SiO 2 , Al 2 O 3 , Fe 2 O 3 ) and minor oxides (MgO, SO 4 , Na 2 O, and K 2 O) in diverse materials (raw material, raw meal, additives, clinker, and types of cement) in cement manufacturing. The FTIR spectroscopy based multivariate models were generated by taking X-ray fluorescence (XRF) as a reference method. Among a number of spectral preprocessing methods, extended multiplicative scatter correction (EMSC) yielded the best PLS models. The standard error of prediction (SEP) for the optimal FTIR based PLS models ranged from 0.10 to 2.07 (w/w%), and the regression coefficient (R 2 ) ranged from 0.95 to 0.99 for PLS predicted vs XRF reference plots. Statistical evaluation of the both methods was carried out by paired t-test at the 95% confidence level and the results showed that the FTIR-ATR combined with PLS model results are consistent with the XRF reference measurements for all the oxides studied. Compared to the XRF method, which can take anywhere from a few minutes to an hour for each measurement, the proposed method is faster, cheaper, and safer. The presented technology also allows rapid monitoring of a cement factory production line.
{"title":"Development of chemometrics method based on infrared spectroscopy for the determination of cement composition and process optimization","authors":"D. Ozdemir, Dilek Tepeli, M. Gümüş","doi":"10.25135/jcm.76.2210.2601","DOIUrl":"https://doi.org/10.25135/jcm.76.2210.2601","url":null,"abstract":": In combination with a multivariate calibration method, FTIR-ATR spectroscopy was presented as a rapid method for the determination of some major oxides (CaO, SiO 2 , Al 2 O 3 , Fe 2 O 3 ) and minor oxides (MgO, SO 4 , Na 2 O, and K 2 O) in diverse materials (raw material, raw meal, additives, clinker, and types of cement) in cement manufacturing. The FTIR spectroscopy based multivariate models were generated by taking X-ray fluorescence (XRF) as a reference method. Among a number of spectral preprocessing methods, extended multiplicative scatter correction (EMSC) yielded the best PLS models. The standard error of prediction (SEP) for the optimal FTIR based PLS models ranged from 0.10 to 2.07 (w/w%), and the regression coefficient (R 2 ) ranged from 0.95 to 0.99 for PLS predicted vs XRF reference plots. Statistical evaluation of the both methods was carried out by paired t-test at the 95% confidence level and the results showed that the FTIR-ATR combined with PLS model results are consistent with the XRF reference measurements for all the oxides studied. Compared to the XRF method, which can take anywhere from a few minutes to an hour for each measurement, the proposed method is faster, cheaper, and safer. The presented technology also allows rapid monitoring of a cement factory production line.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2022-12-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46107079","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 : 2022-12-15DOI: 10.25135/jcm.77.2208.2546
Avani Chokshi, R. Prajapati, Pritesh Desai, Niraj Vyas
: The present study shows the compilation of the results obtained for a very simple, fast and precise high-performance thin-layer chromatography (HPTLC) - densitometric determination of chlorthalidone (CHL), metoprolol succinate ( MET) and telmisartan ( TEL) in bulk drugs as well as the commercially available formulation. The chromatographic separation of samples was performed on Silica Gel 60 F254 aluminum sheets using Toluene: Methanol: Ethyl acetate: Tri-ethylamine as the mobile phase in the volume ratio 4:0.8:1: 1.2. The densitometric scanning was performed at 225 nm wavelength using CAMAG TLC Scanner- IV. The mentioned chromatographic system showed the compact band and symmetrical peaks of CHL, MET and TEL with 0.40 (±0.2), 0.69 (±0.2) and 0.27 (±0.2) retardation factor (Rf) respectively. The reported method is linear in the concentration range of 500-2000 ng/band, 1000-4000 ng/band and 1600-6400 ng/band while the recovery was found in the range of 98.94-99.62%, 98.26-98.41% and 99.86-100.28% for CHL, MET and TEL respectively. The method assayed the marketed formulation with 99.89 (±0.91) for CHL, 98.92 (±1.07) for MET and 100.12 (±0.65) for TEL concerning the label claim. All the results suggested the agreement of the developed method to the ICH Q2(R1) guidelines and its applicability for day-to-day analysis of these drugs in combined pharmaceutical formulations.
{"title":"HPTLC- Densitometric method for assay of chlorthalidone, metoprolol succinate and telmisartan in combined pharmaceutical formulation","authors":"Avani Chokshi, R. Prajapati, Pritesh Desai, Niraj Vyas","doi":"10.25135/jcm.77.2208.2546","DOIUrl":"https://doi.org/10.25135/jcm.77.2208.2546","url":null,"abstract":": The present study shows the compilation of the results obtained for a very simple, fast and precise high-performance thin-layer chromatography (HPTLC) - densitometric determination of chlorthalidone (CHL), metoprolol succinate ( MET) and telmisartan ( TEL) in bulk drugs as well as the commercially available formulation. The chromatographic separation of samples was performed on Silica Gel 60 F254 aluminum sheets using Toluene: Methanol: Ethyl acetate: Tri-ethylamine as the mobile phase in the volume ratio 4:0.8:1: 1.2. The densitometric scanning was performed at 225 nm wavelength using CAMAG TLC Scanner- IV. The mentioned chromatographic system showed the compact band and symmetrical peaks of CHL, MET and TEL with 0.40 (±0.2), 0.69 (±0.2) and 0.27 (±0.2) retardation factor (Rf) respectively. The reported method is linear in the concentration range of 500-2000 ng/band, 1000-4000 ng/band and 1600-6400 ng/band while the recovery was found in the range of 98.94-99.62%, 98.26-98.41% and 99.86-100.28% for CHL, MET and TEL respectively. The method assayed the marketed formulation with 99.89 (±0.91) for CHL, 98.92 (±1.07) for MET and 100.12 (±0.65) for TEL concerning the label claim. All the results suggested the agreement of the developed method to the ICH Q2(R1) guidelines and its applicability for day-to-day analysis of these drugs in combined pharmaceutical formulations.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2022-12-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48797262","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 : 2022-12-01DOI: 10.25135/jcm.73.2210.2591
Ibrahim F. Tahoun, M. Gab-Allah
: The pure materials play a pivotal role in controlling the quality of pharmaceutical products, ensuring comparability and metrological traceability of test results, and performance evaluation of measuring instruments. Herein, the purity characterization of chronic hepatitis C virus sofosbuvir and ledipasvir pharmaceuticals was established based on the assessment of mass fractions of potential impurities in the material including heavy metals, residual solvents, and water content, as well as structurally related organic impurities. The combined estimate of these impurities by mass balance approach led to indirect purity determination of sofosbuvir and ledipasvir materials. The impurities mass fractions in each material were assigned by validated chromatographic methods, Karl Fisher titrator, and inductively coupled plasma-based method. The certified purity values of sofosbuvir and ledipasvir and their corresponding expanded uncertainties (k =2.0 at 95% CL) were found (99.79±0.03) %, (99.69±0.04) %, respectively. The developed certified reference materials (CRMs) with small uncertainty values will support pharmaceutical testing laboratories in their efforts to maintain and improve the quality of results and provide them with high-order CRMs for the accurate determination of both analytes in raw materials and finished products.
{"title":"Development of ledipasvir and sofosbuvir pure certified reference materials for improving quality of pharmaceutical analysis","authors":"Ibrahim F. Tahoun, M. Gab-Allah","doi":"10.25135/jcm.73.2210.2591","DOIUrl":"https://doi.org/10.25135/jcm.73.2210.2591","url":null,"abstract":": The pure materials play a pivotal role in controlling the quality of pharmaceutical products, ensuring comparability and metrological traceability of test results, and performance evaluation of measuring instruments. Herein, the purity characterization of chronic hepatitis C virus sofosbuvir and ledipasvir pharmaceuticals was established based on the assessment of mass fractions of potential impurities in the material including heavy metals, residual solvents, and water content, as well as structurally related organic impurities. The combined estimate of these impurities by mass balance approach led to indirect purity determination of sofosbuvir and ledipasvir materials. The impurities mass fractions in each material were assigned by validated chromatographic methods, Karl Fisher titrator, and inductively coupled plasma-based method. The certified purity values of sofosbuvir and ledipasvir and their corresponding expanded uncertainties (k =2.0 at 95% CL) were found (99.79±0.03) %, (99.69±0.04) %, respectively. The developed certified reference materials (CRMs) with small uncertainty values will support pharmaceutical testing laboratories in their efforts to maintain and improve the quality of results and provide them with high-order CRMs for the accurate determination of both analytes in raw materials and finished products.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2022-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48173945","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 : 2022-10-16DOI: 10.25135/jcm.72.2208.2545
Sagar Patel, C. Patel, J. Surati, A. Akabari, K. Shah
: Two simple, selective, precise, and accurate chromatographic methods, namely reversed-phase high-performance liquid chromatography (RP-HPLC) method and High-performance thin-layer chromatography (HPTLC), were developed and validated for the simultaneous determination of Atorvastatin (ATO) and Perindopril (PER). The developed HPTLC method was used for the separation and quantitation of the studied drugs on silica gel 60F254 TLC plates. Dichloromethane: Methanol: Ethyl acetate: Glacial acetic acid (6:2:2:0.1, v/v/v/v) was used as a developing system and the separated bands were UV-scanned at 221 nm. Linear relationships were obtained in the range of 800 – 4800 ng/band for Atorvastatin and 200 – 1200 ng/band for Perindopril with a regression coefficient greater than 0.999. The Rf value of the drug was found to be 0.70 ± 0.02 and 0.39 ± 0.03 for Atorvastatin and Perindopril respectively. The developed RP-HPLC depended on chromatographic separation of the studied drugs on a C18 column using Acetonitrile: Methanol: Potassium dihydrogen orthophosphate (pH 3 adjusted with orthophosphoric acid) ((40:10:50), v/v/v) as a mobile phase delivered at a constant flow rate of 1 mL/min with UV detection at 240 nm. The calibration curves were linear (r2 > 0.999) over the concentration range 20-100 µg/mL for Atorvastatin and 10-50µg/mL for Perindopril. The average retention times for Atorvastatin and Perindopril were 3.42 and 8.92 min, respectively. Factors affecting the developed methods have been studied and optimized. Further, methods validation has been carried out according to ICH guidelines. The proposed methods were successfully applied for the determination of the studied drug simultaneously in bulk and synthetic mixture qualitatively and quantitatively. Statistical analysis by the F test showed no significant difference between the results obtained by the two methods. The uncertainty measurement was also carried out for the quantification of both components. The proposed HPTLC method proved to be more sensitive, while the HPLC gave more reproducible results and was time-saving.
{"title":"Validated chromatographic methods for concurrent determination of atorvastatin and perindopril","authors":"Sagar Patel, C. Patel, J. Surati, A. Akabari, K. Shah","doi":"10.25135/jcm.72.2208.2545","DOIUrl":"https://doi.org/10.25135/jcm.72.2208.2545","url":null,"abstract":": Two simple, selective, precise, and accurate chromatographic methods, namely reversed-phase high-performance liquid chromatography (RP-HPLC) method and High-performance thin-layer chromatography (HPTLC), were developed and validated for the simultaneous determination of Atorvastatin (ATO) and Perindopril (PER). The developed HPTLC method was used for the separation and quantitation of the studied drugs on silica gel 60F254 TLC plates. Dichloromethane: Methanol: Ethyl acetate: Glacial acetic acid (6:2:2:0.1, v/v/v/v) was used as a developing system and the separated bands were UV-scanned at 221 nm. Linear relationships were obtained in the range of 800 – 4800 ng/band for Atorvastatin and 200 – 1200 ng/band for Perindopril with a regression coefficient greater than 0.999. The Rf value of the drug was found to be 0.70 ± 0.02 and 0.39 ± 0.03 for Atorvastatin and Perindopril respectively. The developed RP-HPLC depended on chromatographic separation of the studied drugs on a C18 column using Acetonitrile: Methanol: Potassium dihydrogen orthophosphate (pH 3 adjusted with orthophosphoric acid) ((40:10:50), v/v/v) as a mobile phase delivered at a constant flow rate of 1 mL/min with UV detection at 240 nm. The calibration curves were linear (r2 > 0.999) over the concentration range 20-100 µg/mL for Atorvastatin and 10-50µg/mL for Perindopril. The average retention times for Atorvastatin and Perindopril were 3.42 and 8.92 min, respectively. Factors affecting the developed methods have been studied and optimized. Further, methods validation has been carried out according to ICH guidelines. The proposed methods were successfully applied for the determination of the studied drug simultaneously in bulk and synthetic mixture qualitatively and quantitatively. Statistical analysis by the F test showed no significant difference between the results obtained by the two methods. The uncertainty measurement was also carried out for the quantification of both components. The proposed HPTLC method proved to be more sensitive, while the HPLC gave more reproducible results and was time-saving.","PeriodicalId":15343,"journal":{"name":"Journal of Chemical Metrology","volume":" ","pages":""},"PeriodicalIF":1.3,"publicationDate":"2022-10-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47491515","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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