Lenalidomide is a drug that has immune-modulating, anti-angiogenic, and anti-inflammatory properties. In this study, we developed green HPLC and spectrophotometric methods to determine the concentration of lenalidomide in pure and pharmaceutical formulations. In the HPLC method, 10 mM potassium dihydrogen phosphate solution (pH: 2.0) and ethanol (50:50, V/V) were used as mobile phases, isocratic elution was applied at a flow rate of 1.0 mL min−1 and detection was made at 304 nm. In the spectrophotometric method, the spectral patterns of standard solutions in different solvents were comprehensively examined, the best spectra were obtained with ultrapure water, and a wavelength of 304 nm was selected for detection. Both methods have been validated according to ICH guidelines for various parameters. Correlation coefficients greater than 0.999 were determined for both methods in the concentration range of 5–30 μg mL−1. The developed methods were applied to commercial formulations, and comparisons of the results were made using the Student (t) test for means and the Fischer (F) test for standard deviations. No statistically significant difference was observed between the methods. The greenness evaluation of these methods was carried out using AGREE software. The developed methods are proposed as excellent environmental and operator-friendly alternatives for the quantification of Lenalidomide in pharmaceutical formulations.
来那度胺是一种具有免疫调节、抗血管生成和抗炎特性的药物。本研究开发了绿色高效液相色谱法和分光光度法来测定来那度胺在纯品和药物制剂中的浓度。高效液相色谱法以 10 mM 磷酸二氢钾溶液（pH：2.0）和乙醇（50:50, V/V）为流动相，等度洗脱，流速为 1.0 mL min-1，检测波长为 304 nm。在分光光度法中，对不同溶剂中标准溶液的光谱图进行了综合考察，用超纯水得到了最佳光谱，并选择 304 nm 波长进行检测。这两种方法都根据 ICH 指南对各种参数进行了验证。在 5-30 μg mL-1 的浓度范围内，两种方法的相关系数均大于 0.999。将所开发的方法应用于商业制剂，并使用学生（t）检验（均值）和费舍尔（F）检验（标准偏差）对结果进行比较。结果表明，这些方法之间没有明显的统计学差异。使用 AGREE 软件对这些方法进行了绿色评估。建议采用所开发的方法来定量检测药物制剂中的来那度胺，这些方法既环保又便于操作。
{"title":"Development, validation and greenness assessment of environmentally friendly analytical methods for the quantification of lenalidomide in pharmaceutical formulations","authors":"İbrahim Demir, I. Bulduk, Hüseyin Enginar","doi":"10.1556/1326.2023.01185","DOIUrl":"https://doi.org/10.1556/1326.2023.01185","url":null,"abstract":"Lenalidomide is a drug that has immune-modulating, anti-angiogenic, and anti-inflammatory properties. In this study, we developed green HPLC and spectrophotometric methods to determine the concentration of lenalidomide in pure and pharmaceutical formulations. In the HPLC method, 10 mM potassium dihydrogen phosphate solution (pH: 2.0) and ethanol (50:50, V/V) were used as mobile phases, isocratic elution was applied at a flow rate of 1.0 mL min−1 and detection was made at 304 nm. In the spectrophotometric method, the spectral patterns of standard solutions in different solvents were comprehensively examined, the best spectra were obtained with ultrapure water, and a wavelength of 304 nm was selected for detection. Both methods have been validated according to ICH guidelines for various parameters. Correlation coefficients greater than 0.999 were determined for both methods in the concentration range of 5–30 μg mL−1. The developed methods were applied to commercial formulations, and comparisons of the results were made using the Student (t) test for means and the Fischer (F) test for standard deviations. No statistically significant difference was observed between the methods. The greenness evaluation of these methods was carried out using AGREE software. The developed methods are proposed as excellent environmental and operator-friendly alternatives for the quantification of Lenalidomide in pharmaceutical formulations.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-12-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138950048","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}
N. Nakov, L. Anastasova, Marija Zafirova Gjorgievska, J. Acevska, K. Brezovska, R. Petkovska, A. Dimitrovska
In this study, two different ethanol-based RP-HPLC methods for assay and quantification of rivaroxaban related substances in tablets were developed, based on green analytical chemistry (GAC) principles, using the design of experiments approach. The chromatographic separation was performed on X-Bridge C18 column (250 × 4.6 mm, 5 µm particle size), using isocratic elution with ethanol : water (35:65, % v/v) for the assay and gradient elution with ethanol/water mobile phase, for related substances, with a flow rate of 1.0 mL min−1. The gradient method was optimized for the separation of three specified impurities (impurity G, impurity H, and impurity 14) and the selectivity was further confirmed using forced degradation studies. Both methods were validated in accordance with ICH guidelines. The robustness of the methods was confirmed with the Central Composite Face Design of Experiments. Analytical Eco-scale approach and AGREE metrics confirmed that both methods are in accordance with the GAC principles. The proposed ethanol-based RP-HPLC methods were applied for assay and determination of related substances in rivaroxaban 10 mg tablets obtained from three different manufacturers available on the Macedonian market.
{"title":"Green RP-HPLC methods for assay and related substances in rivaroxaban tablets","authors":"N. Nakov, L. Anastasova, Marija Zafirova Gjorgievska, J. Acevska, K. Brezovska, R. Petkovska, A. Dimitrovska","doi":"10.1556/1326.2023.01178","DOIUrl":"https://doi.org/10.1556/1326.2023.01178","url":null,"abstract":"In this study, two different ethanol-based RP-HPLC methods for assay and quantification of rivaroxaban related substances in tablets were developed, based on green analytical chemistry (GAC) principles, using the design of experiments approach. The chromatographic separation was performed on X-Bridge C18 column (250 × 4.6 mm, 5 µm particle size), using isocratic elution with ethanol : water (35:65, % v/v) for the assay and gradient elution with ethanol/water mobile phase, for related substances, with a flow rate of 1.0 mL min−1. The gradient method was optimized for the separation of three specified impurities (impurity G, impurity H, and impurity 14) and the selectivity was further confirmed using forced degradation studies. Both methods were validated in accordance with ICH guidelines. The robustness of the methods was confirmed with the Central Composite Face Design of Experiments. Analytical Eco-scale approach and AGREE metrics confirmed that both methods are in accordance with the GAC principles. The proposed ethanol-based RP-HPLC methods were applied for assay and determination of related substances in rivaroxaban 10 mg tablets obtained from three different manufacturers available on the Macedonian market.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-11-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139212708","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}
Burhan Ceylan, Gizem Tırıs, Ş. E. KEPEKÇİ TEKKELİ, C. Önal, A. Önal
A novel simple and cost effective HPLC technique was presented for the quantification of selexipag (SLP) in human plasma sample and the technique's applicability to a pharmacokinetic investigation. Chromatographic separation was achieved with C18 (5 µm × 4.6 mm × 150 mm) column, at 30 °C with isocratic elution, mobile phase composed of solution A (acetonitrile), and solution B (0.5% formic acid) (65:35 v/v) at flow rate 1.2 mL min−1. The linearity range is 10–150 ng mL−1. As sample preparation step human plasma was precipitated with acetonitrile and the detection was provided at 300 nm. The retention time is 8.20 ± 0.02 min. LOD is found to be 3.3 ng mL−1 for drug. The method was applied to the analysis of SLP in human plasma with good recovery as 97.83%. Validation of the studied methods was carried out according to EMA guideline. The new method applied on a prototype pharmacokinetic study by administration of 800 μg SLP to a healthy volunteer and parameters like AUC0–24, AUC0–∞, Cmax, tmax, and t1/2 were assessed.
{"title":"A novel HPLC method for selexipag in human plasma and application to a prototype pharmacokinetic study","authors":"Burhan Ceylan, Gizem Tırıs, Ş. E. KEPEKÇİ TEKKELİ, C. Önal, A. Önal","doi":"10.1556/1326.2023.01167","DOIUrl":"https://doi.org/10.1556/1326.2023.01167","url":null,"abstract":"A novel simple and cost effective HPLC technique was presented for the quantification of selexipag (SLP) in human plasma sample and the technique's applicability to a pharmacokinetic investigation. Chromatographic separation was achieved with C18 (5 µm × 4.6 mm × 150 mm) column, at 30 °C with isocratic elution, mobile phase composed of solution A (acetonitrile), and solution B (0.5% formic acid) (65:35 v/v) at flow rate 1.2 mL min−1. The linearity range is 10–150 ng mL−1. As sample preparation step human plasma was precipitated with acetonitrile and the detection was provided at 300 nm. The retention time is 8.20 ± 0.02 min. LOD is found to be 3.3 ng mL−1 for drug. The method was applied to the analysis of SLP in human plasma with good recovery as 97.83%. Validation of the studied methods was carried out according to EMA guideline. The new method applied on a prototype pharmacokinetic study by administration of 800 μg SLP to a healthy volunteer and parameters like AUC0–24, AUC0–∞, Cmax, tmax, and t1/2 were assessed.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-11-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139245710","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}
Di Cao, Haishan Long, Xuebin Shen, Bin Hu, Shixia Xu, Huining Zhang, Zhongxiang Zhao, Jun Han
Atractylodis macrocephalae rhizome (AMR) belongs to medicine food homology. Its' clinical application of invigorating the spleen-stomach of AMR was applied to various diseases. In this research, a UPLC-QTOF-MS method was developed for qualitative and quantitative analysis of AMR, simultaneously. A Waters Acquity BEH C18 column (2.1 mm × 100 mm, 1.7 μm particle size) was used for separation of AMR multi-components. The column was eluted with a mobile phase of 0.1% formic acid-water and 0.1% formic acid-acetonitrile. Electron spray ionization with positive-ion mode and external standard method was utilized for quantifying the nine analytes in AMR. Constituents of AMR were scanned by UPLC-QTOF-MS and then identified by mass fragments and chromatographic information compared with the published literature and reference standards. Under positive mode, a total of 61 chemical compositions including 16 terpenoids, 8 polyacetylenes, 6 aromatics, 5 flavonoids, 5 coumarins, 5 organic acids, 4 amino acids, 3 fatty acids, 3 aliphatics, 2 steroids, and 2 alkenes, a nucleoside and an aldehyde were identified. Simultaneously, the contents of three amino acids (L-tyrosine, L-phenylalanine, and L-tryptophan), three sesquiterpenoids (atractylenolide Ⅲ, atractylenolide Ⅱ, and atractylenolide Ⅰ), a flavonoid (rutin), an organic acid (ferulic acid), and a pentacyclic triterpenoid (oleanolic acid) were determined in seventeen AMR batches. Amino acids and triterpenoid were quantified for the first time in AMR. The UPLC-QTOF-MS method developed in this article was reliable, practical, and useful for qualitative and quantitative evaluation of AMR multi-components.
白术属药食同源植物。白术具有健脾和胃的功效，临床应用于多种疾病。本研究建立了一种UPLC-QTOF-MS方法，可同时对AMR进行定性和定量分析。采用Waters Acquity BEH C18色谱柱（2.1 mm × 100 mm，1.7 μm粒径）分离AMR多组分。以 0.1% 甲酸-水和 0.1% 甲酸-乙腈为流动相进行洗脱。采用正离子模式电子喷雾电离和外标法对 AMR 中的 9 种分析物进行定量。采用 UPLC-QTOF-MS 对 AMR 中的成分进行扫描，然后根据质量碎片和色谱信息与已发表的文献和参考标准进行比对鉴定。在阳性模式下，共鉴定出 61 种化学成分，包括 16 种萜类化合物、8 种多乙炔类化合物、6 种芳香族化合物、5 种黄酮类化合物、5 种香豆素类化合物、5 种有机酸类化合物、4 种氨基酸类化合物、3 种脂肪酸类化合物、3 种脂肪类化合物、2 种甾体类化合物、2 种烯类化合物、1 种核苷类化合物和 1 种醛类化合物。同时，三种氨基酸（L-酪氨酸、L-苯丙氨酸和 L-色氨酸）、三种倍半萜类化合物（苍术内酯 Ⅲ、苍术内酯 Ⅱ、和白术内酯Ⅰ）、一种黄酮类化合物（芦丁）、一种有机酸（阿魏酸）和一种五环三萜类化合物（齐墩果酸）。在 AMR 中首次对氨基酸和三萜类化合物进行了定量。本文开发的 UPLC-QTOF-MS 方法可靠、实用，可用于 AMR 多成分的定性和定量评价。
{"title":"Simultaneous qualitative and quantitative analysis for evaluating constituents of Atractylodis macrocephalae rhizome by UPLC-QTOF-MS","authors":"Di Cao, Haishan Long, Xuebin Shen, Bin Hu, Shixia Xu, Huining Zhang, Zhongxiang Zhao, Jun Han","doi":"10.1556/1326.2023.01151","DOIUrl":"https://doi.org/10.1556/1326.2023.01151","url":null,"abstract":"Atractylodis macrocephalae rhizome (AMR) belongs to medicine food homology. Its' clinical application of invigorating the spleen-stomach of AMR was applied to various diseases. In this research, a UPLC-QTOF-MS method was developed for qualitative and quantitative analysis of AMR, simultaneously. A Waters Acquity BEH C18 column (2.1 mm × 100 mm, 1.7 μm particle size) was used for separation of AMR multi-components. The column was eluted with a mobile phase of 0.1% formic acid-water and 0.1% formic acid-acetonitrile. Electron spray ionization with positive-ion mode and external standard method was utilized for quantifying the nine analytes in AMR. Constituents of AMR were scanned by UPLC-QTOF-MS and then identified by mass fragments and chromatographic information compared with the published literature and reference standards. Under positive mode, a total of 61 chemical compositions including 16 terpenoids, 8 polyacetylenes, 6 aromatics, 5 flavonoids, 5 coumarins, 5 organic acids, 4 amino acids, 3 fatty acids, 3 aliphatics, 2 steroids, and 2 alkenes, a nucleoside and an aldehyde were identified. Simultaneously, the contents of three amino acids (L-tyrosine, L-phenylalanine, and L-tryptophan), three sesquiterpenoids (atractylenolide Ⅲ, atractylenolide Ⅱ, and atractylenolide Ⅰ), a flavonoid (rutin), an organic acid (ferulic acid), and a pentacyclic triterpenoid (oleanolic acid) were determined in seventeen AMR batches. Amino acids and triterpenoid were quantified for the first time in AMR. The UPLC-QTOF-MS method developed in this article was reliable, practical, and useful for qualitative and quantitative evaluation of AMR multi-components.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-11-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139244330","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}
Ahmad A. Deeb, Mohammad Abuothman, Mohammad Hailat, Omar Abuyaman, Ruba K. Albizreh
Coloring agents in foods and drinks have been popular for centuries. This study aims to analyze the presence of ten synthetic colors (namely, (allura red (E129), amaranth (E123), sunset yellow (E110), tetrazine (E102), fast green (E143), ponceau 4R (New Coccine) (E124), erythrosin B (E127), brilliant blue FCF (E133), brilliant black (E151) and carmoisine (E122))) in food and drink samples using ultra-high-performance liquid chromatography diode array detection (UHPLC-DAD). The present analytical method was carried out using Agilent Poroshell 120 HPH-C18 column, 3 × 100 mm, 2.7 µm, and a mobile phase consisting of 10 mM Na2HPO4, pH 7, mixed with methanol as a time-increment gradient solution until the time was 20 min, then decreased with time until the time was 26 min. The pH was set by orthophosphoric acid at 7 and 5 μL injection volume, 0.50 mL flow rate, and the elution systems were monitored at 428 nm for E102, 518 nm for E124, E110, E129, E122, 530 nm for E151, E127, 622 nm for E143, and E133, respectively. The limit of detection and quantification for all colors ranged from 0.017 to 0.025 and 0.057 and 0.082 mg L−1, respectively. The correlation coefficient values ranged between 0.9991 and 1.0. The selectivity of the assay revealed no interference from other components in the analyzed samples. The percent recovery and precision (intra- and inter-day) of the spiked samples were within the acceptable limits of the ICH guidelines. Five analytical parameters were employed, and the results showed a new, novel, and robust method according to ICH guidelines for analyzing these colors. While most of the investigated food and drinks fell within the accepted range, some fell outside. The current sample preparation and analytical methods are comprehensive and universal for extracting and measuring synthetic colors in various food and drink samples.
{"title":"Analyzing the presence of ten synthetic colors in selected food and drink samples using ultra high-performance liquid chromatography diode array detection analysis","authors":"Ahmad A. Deeb, Mohammad Abuothman, Mohammad Hailat, Omar Abuyaman, Ruba K. Albizreh","doi":"10.1556/1326.2023.01175","DOIUrl":"https://doi.org/10.1556/1326.2023.01175","url":null,"abstract":"Coloring agents in foods and drinks have been popular for centuries. This study aims to analyze the presence of ten synthetic colors (namely, (allura red (E129), amaranth (E123), sunset yellow (E110), tetrazine (E102), fast green (E143), ponceau 4R (New Coccine) (E124), erythrosin B (E127), brilliant blue FCF (E133), brilliant black (E151) and carmoisine (E122))) in food and drink samples using ultra-high-performance liquid chromatography diode array detection (UHPLC-DAD). The present analytical method was carried out using Agilent Poroshell 120 HPH-C18 column, 3 × 100 mm, 2.7 µm, and a mobile phase consisting of 10 mM Na2HPO4, pH 7, mixed with methanol as a time-increment gradient solution until the time was 20 min, then decreased with time until the time was 26 min. The pH was set by orthophosphoric acid at 7 and 5 μL injection volume, 0.50 mL flow rate, and the elution systems were monitored at 428 nm for E102, 518 nm for E124, E110, E129, E122, 530 nm for E151, E127, 622 nm for E143, and E133, respectively. The limit of detection and quantification for all colors ranged from 0.017 to 0.025 and 0.057 and 0.082 mg L−1, respectively. The correlation coefficient values ranged between 0.9991 and 1.0. The selectivity of the assay revealed no interference from other components in the analyzed samples. The percent recovery and precision (intra- and inter-day) of the spiked samples were within the acceptable limits of the ICH guidelines. Five analytical parameters were employed, and the results showed a new, novel, and robust method according to ICH guidelines for analyzing these colors. While most of the investigated food and drinks fell within the accepted range, some fell outside. The current sample preparation and analytical methods are comprehensive and universal for extracting and measuring synthetic colors in various food and drink samples.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-11-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139246840","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}
Abstract An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of monocrotaline and usaramine in rat plasma, to study the plasma drug concentration and pharmacokinetics, and to calculate the absolute bioavailability. The plasma was treated with acetonitrile and methanol (9:1, v/v) protein precipitation method. The chromatographic column was UPLC HSS T3 (50 mm × 2.1 mm, 1.7 μm), the mobile phase was methanol-water (containing 0.1% formic acid with 10 mM ammonium acetate in water), and the elution time was 4 min at a flow rate of 0.4 mL min −1 . Electrospray ionization (ESI) positive ion mode was used for detection and multiple reaction monitoring (MRM) mode was used for quantitative analysis. Monocrotaline and usaramine were administered sublingual intravenously (iv) 1 mg kg −1 and orally (po) 5 mg kg −1 , respectively, with 6 rats in each group, for a total of 24 rats. Then the pharmacokinetic differences in rats were evaluated. For the UPLC-MS/MS method, the calibration curve showed good linearity in the range of 2–2,000 ng mL −1 , where r was greater than 0.99. The precision, accuracy, recovery, matrix effect and stability results were all consistent with the requirements of biological sample detection methods. to provide scientific experimental basis for the basic research The bioavailability of monocrotaline and usaramine in rat plasma was calculated, which was 43.5 and 19.5%, respectively.
摘要建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)测定大鼠血浆中苦参碱和乌萨拉明的方法，研究其血药浓度和药代动力学，并计算绝对生物利用度。血浆用乙腈-甲醇(9:1,v/v)蛋白沉淀法处理。色谱柱为UPLC HSS T3 (50 mm × 2.1 mm, 1.7 μm)，流动相为甲醇-水(含0.1%甲酸和10 mm乙酸铵)，洗脱时间为4 min，流速为0.4 mL min−1。采用电喷雾电离(ESI)正离子模式进行检测，多反应监测(MRM)模式进行定量分析。分别舌下静脉注射(iv) 1 mg kg - 1和口服(po) 5 mg kg - 1，每组6只大鼠，共24只大鼠。然后评价其在大鼠体内的药动学差异。UPLC-MS/MS方法在2 ~ 2000 ng mL−1范围内线性良好，其中r > 0.99;精密度、准确度、回收率、基质效应和稳定性结果均符合生物样品检测方法的要求。为基础研究提供科学的实验依据。计算了大鼠血浆中苦杏仁碱和乌苏胺的生物利用度，分别为43.5%和19.5%。
{"title":"Determination of monocrotaline and usaramine in rat plasma by UPLC-MS/MS and their pharmacokinetics","authors":"Fan Chen, Ziyue Wang, Xiaoyun Xia, Wanhang Wang, Yizhe Ma, Xiuwei Shen, Xuzhao Zhou, Congcong Wen","doi":"10.1556/1326.2023.01160","DOIUrl":"https://doi.org/10.1556/1326.2023.01160","url":null,"abstract":"Abstract An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of monocrotaline and usaramine in rat plasma, to study the plasma drug concentration and pharmacokinetics, and to calculate the absolute bioavailability. The plasma was treated with acetonitrile and methanol (9:1, v/v) protein precipitation method. The chromatographic column was UPLC HSS T3 (50 mm × 2.1 mm, 1.7 μm), the mobile phase was methanol-water (containing 0.1% formic acid with 10 mM ammonium acetate in water), and the elution time was 4 min at a flow rate of 0.4 mL min −1 . Electrospray ionization (ESI) positive ion mode was used for detection and multiple reaction monitoring (MRM) mode was used for quantitative analysis. Monocrotaline and usaramine were administered sublingual intravenously (iv) 1 mg kg −1 and orally (po) 5 mg kg −1 , respectively, with 6 rats in each group, for a total of 24 rats. Then the pharmacokinetic differences in rats were evaluated. For the UPLC-MS/MS method, the calibration curve showed good linearity in the range of 2–2,000 ng mL −1 , where r was greater than 0.99. The precision, accuracy, recovery, matrix effect and stability results were all consistent with the requirements of biological sample detection methods. to provide scientific experimental basis for the basic research The bioavailability of monocrotaline and usaramine in rat plasma was calculated, which was 43.5 and 19.5%, respectively.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-11-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"134954265","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}
Roza Linda, Wida Maya Mustika, Mohamad Rafi, Eti Rohaeti, Lee Wah Lim
Abstract Silica, as a stationary phase, has low separation efficiency accompanied by overlapping, broadened, and tailed peaks, so it needs to be modified to improve its efficiency. This study aims to develop a silica-based stationary phase modified by tetraethylene glycol (TEG) to separate phenolic compounds. Silica was modified by a chemical bond between silanol groups on the silica surface and TEG through a 3-glycidyloxypropylmethoxysilane reaction. The modified silica was packed into a capillary column and used to separate simple phenolic compounds consisting of phenol, pyrocatechol, and pyrogallol. A sample of 0.2 µL was injected into the capillary liquid chromatography and the mobile phase employed was acetonitrile 98% with a flow rate of 3 μL min −1 . Elution was also done isocratically in this process and detection was carried out at a wavelength of 254 nm. The mixture of simple phenolic compounds was successfully separated in less than 7 min. The asymmetry factor and resolution were 1.43–2.12 and 1.72–5.43 respectively. The number of the theoretical plates ranged from 213 to 7,857. Columns containing Si-TEG stationary phase also separate phenolic compounds, which consist of gallic acid, syringic acid, ferulic acid, and caffeic acid. A sample of 0.2 µL was injected into the capillary liquid chromatography and successfully separated the mixture in less than 12 min. The samples were eluted isocratically using a mixture of methanol and 50 mM phosphate buffer pH 2.5 (8:92) with a flow rate of 3 μL min −1 . The phenolic acids compounds were detected at a wavelength of 280 nm. The chromatogram showed four separate peaks. The asymmetry factor and resolution were 1.53–1.63 and 1.14–1.74, respectively, but the number of the theoretical plates was low, ranging from 190 to 796.
{"title":"A stationary phase of tetraethylene glycol-modified silica for separation of phenolic acids","authors":"Roza Linda, Wida Maya Mustika, Mohamad Rafi, Eti Rohaeti, Lee Wah Lim","doi":"10.1556/1326.2023.01131","DOIUrl":"https://doi.org/10.1556/1326.2023.01131","url":null,"abstract":"Abstract Silica, as a stationary phase, has low separation efficiency accompanied by overlapping, broadened, and tailed peaks, so it needs to be modified to improve its efficiency. This study aims to develop a silica-based stationary phase modified by tetraethylene glycol (TEG) to separate phenolic compounds. Silica was modified by a chemical bond between silanol groups on the silica surface and TEG through a 3-glycidyloxypropylmethoxysilane reaction. The modified silica was packed into a capillary column and used to separate simple phenolic compounds consisting of phenol, pyrocatechol, and pyrogallol. A sample of 0.2 µL was injected into the capillary liquid chromatography and the mobile phase employed was acetonitrile 98% with a flow rate of 3 μL min −1 . Elution was also done isocratically in this process and detection was carried out at a wavelength of 254 nm. The mixture of simple phenolic compounds was successfully separated in less than 7 min. The asymmetry factor and resolution were 1.43–2.12 and 1.72–5.43 respectively. The number of the theoretical plates ranged from 213 to 7,857. Columns containing Si-TEG stationary phase also separate phenolic compounds, which consist of gallic acid, syringic acid, ferulic acid, and caffeic acid. A sample of 0.2 µL was injected into the capillary liquid chromatography and successfully separated the mixture in less than 12 min. The samples were eluted isocratically using a mixture of methanol and 50 mM phosphate buffer pH 2.5 (8:92) with a flow rate of 3 μL min −1 . The phenolic acids compounds were detected at a wavelength of 280 nm. The chromatogram showed four separate peaks. The asymmetry factor and resolution were 1.53–1.63 and 1.14–1.74, respectively, but the number of the theoretical plates was low, ranging from 190 to 796.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-11-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"136348430","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}
Abstract Pinus merkusii Jungh & De Vries. has become increasingly gathered more attention from researchers because the plant has a range of folk medicinal uses. Heartwood plant is the major source of dehydroabietic acid (DHAA) and abietic acid (AA), which possesses several medicinal properties, such as antiviral, antimicrobial, antiobesity and anti-inflammatory. The research proposed herein a low-cost, fast, specific, uncomplicated, sensitive, precise reverse-phase high-performance liquid chromatography (RP-HPLC). This method was conducted and validated for evaluating an amount of DHAA and AA in ethanol extract and oral spray containing P. merkusii heartwood extract. Additionally, stability and antimicrobial activities against clinically isolated Streptococcus mutans of the oral spray were determined. The separation was achieved on Pursuit 200Å PFP column, 150 × 4.6 mm, particles of 3 µm with a flow rate of 1.0 mL min −1 . Methanol and water (70:30 v/v) were used as eluent with an isocratic mode and sample analysis volume was set at 10 µL, at a detection wavelength of 210 and 245 nm. The developed HPLC method for analysis of DHAA and AA showed good linearity with correlation coefficients equal to 1. Moreover, other validation parameters, comprised of accuracy, precision, specificity and detection and quantitation limits of this method displayed excellent reliability, validity and sensitivity. This method could be an interesting alternative for quantitative measurement of P. merkusii heartwood extract, oral spray formulation and other P. merkusii heartwood extract preparations. The result from antibacterial tests suggested that the oral spray containing P. merkusii heartwood extract is able to inhibit the oral pathogens causing dental caries. The oral spray decreased S. mutans population size by about 0.5–2 Log CFU mL −1 at 1–4 h and complete elimination of all bacteria strains within 24 h. This study provides validity for using P. merkusii heartwood extract as an alternative for preventing and treating oral infectious diseases.
{"title":"HPLC-DAD method validation for quantification of dehydroabietic acid and abietic acid in oral spray containing Pinus merkusii heartwood extract and its antibacterial effects on clinically isolated Streptococcus mutans","authors":"Apirak Sakunpak, Worawan Saingam","doi":"10.1556/1326.2023.01149","DOIUrl":"https://doi.org/10.1556/1326.2023.01149","url":null,"abstract":"Abstract Pinus merkusii Jungh & De Vries. has become increasingly gathered more attention from researchers because the plant has a range of folk medicinal uses. Heartwood plant is the major source of dehydroabietic acid (DHAA) and abietic acid (AA), which possesses several medicinal properties, such as antiviral, antimicrobial, antiobesity and anti-inflammatory. The research proposed herein a low-cost, fast, specific, uncomplicated, sensitive, precise reverse-phase high-performance liquid chromatography (RP-HPLC). This method was conducted and validated for evaluating an amount of DHAA and AA in ethanol extract and oral spray containing P. merkusii heartwood extract. Additionally, stability and antimicrobial activities against clinically isolated Streptococcus mutans of the oral spray were determined. The separation was achieved on Pursuit 200Å PFP column, 150 × 4.6 mm, particles of 3 µm with a flow rate of 1.0 mL min −1 . Methanol and water (70:30 v/v) were used as eluent with an isocratic mode and sample analysis volume was set at 10 µL, at a detection wavelength of 210 and 245 nm. The developed HPLC method for analysis of DHAA and AA showed good linearity with correlation coefficients equal to 1. Moreover, other validation parameters, comprised of accuracy, precision, specificity and detection and quantitation limits of this method displayed excellent reliability, validity and sensitivity. This method could be an interesting alternative for quantitative measurement of P. merkusii heartwood extract, oral spray formulation and other P. merkusii heartwood extract preparations. The result from antibacterial tests suggested that the oral spray containing P. merkusii heartwood extract is able to inhibit the oral pathogens causing dental caries. The oral spray decreased S. mutans population size by about 0.5–2 Log CFU mL −1 at 1–4 h and complete elimination of all bacteria strains within 24 h. This study provides validity for using P. merkusii heartwood extract as an alternative for preventing and treating oral infectious diseases.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135935001","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}
İbrahim Demir, İbrahim Bulduk, Hüseyin Enginar, Cemal Çifci
Abstract Mirtazapine is an antidepressant medication used to treat the major depressive disorder in adults. In this study, two different chromatographic methods were developed for the determination of mirtazapine in pharmaceutical products. In the first method, An Extend C 18 column (250 × 4.6 mm, 5 μm) was used and the temperature was kept constant at 25 °C. The mobile phase was determined as 0.1% formic acid solution and acetonitrile (80/20, v/v), and isocratic elution was applied. The flow rate of the mobile phase was determined as 1.0 mL min −1 and the injection volume was 20 µL. Detection was performed at 291 nm. using a UV detector. In the second method, ethanol was used as the organic modifier. The only difference between these methods was the organic modifier. All other conditions of the methods were the same. Both chromatographic methods were validated by ICH guidelines for various parameters such as selectivity, linearity, accuracy, precision, detection and quantification limit, and robustness. The determination coefficients of chromatographic methods were greater than 0.999 in the concentration range of 5–30 µg mL −1 . of mirtazapine. Later, these chromatographic methods were applied to pharmaceutical formulations. Comparison of the obtained results in terms of means was made using Student's ( t ) test, and comparisons in terms of standard deviations were made using the Fischer (F) test. It was observed that there was no significant difference between these methods. These two methods were then evaluated using the AGREE-Analytical GREEnness metric software. The chromatographic method using ethanol as an organic modifier has been proposed as an excellent eco-friendly and analyst-friendly alternative for the determination of mirtazapine in pharmaceutical formulations.
米氮平是一种用于治疗成人重度抑郁症的抗抑郁药物。建立了两种不同的色谱法测定药品中米氮平的含量。第一种方法采用An Extend C 18色谱柱(250 × 4.6 mm, 5 μm)，温度恒定在25℃。流动相为0.1%甲酸溶液-乙腈(80/20,v/v)，等密度洗脱。流动相流速为1.0 mL min - 1，进样量为20µL。在291 nm处检测。使用紫外线探测器。第二种方法以乙醇为有机改性剂。这些方法之间的唯一区别是有机改性剂。所有方法的其他条件相同。两种色谱方法均通过ICH指南验证了各种参数，如选择性、线性、准确度、精密度、检测和定量限以及鲁棒性。在5 ~ 30µg mL−1的浓度范围内，色谱法的测定系数均大于0.999。米氮平。后来，这些色谱方法被应用于药物制剂。采用Student’s (t)检验比较所得结果的均值，采用Fischer (F)检验比较标准差。结果表明，两种方法间无显著性差异。然后使用AGREE-Analytical GREEnness度量软件对这两种方法进行评估。以乙醇为有机改性剂的色谱法是测定药物制剂中米氮平的一种环境友好的方法。
{"title":"A green HPLC method for determination of mirtazapine in pharmaceutical products: Development, validation, and greenness assessment","authors":"İbrahim Demir, İbrahim Bulduk, Hüseyin Enginar, Cemal Çifci","doi":"10.1556/1326.2023.01155","DOIUrl":"https://doi.org/10.1556/1326.2023.01155","url":null,"abstract":"Abstract Mirtazapine is an antidepressant medication used to treat the major depressive disorder in adults. In this study, two different chromatographic methods were developed for the determination of mirtazapine in pharmaceutical products. In the first method, An Extend C 18 column (250 × 4.6 mm, 5 μm) was used and the temperature was kept constant at 25 °C. The mobile phase was determined as 0.1% formic acid solution and acetonitrile (80/20, v/v), and isocratic elution was applied. The flow rate of the mobile phase was determined as 1.0 mL min −1 and the injection volume was 20 µL. Detection was performed at 291 nm. using a UV detector. In the second method, ethanol was used as the organic modifier. The only difference between these methods was the organic modifier. All other conditions of the methods were the same. Both chromatographic methods were validated by ICH guidelines for various parameters such as selectivity, linearity, accuracy, precision, detection and quantification limit, and robustness. The determination coefficients of chromatographic methods were greater than 0.999 in the concentration range of 5–30 µg mL −1 . of mirtazapine. Later, these chromatographic methods were applied to pharmaceutical formulations. Comparison of the obtained results in terms of means was made using Student's ( t ) test, and comparisons in terms of standard deviations were made using the Fischer (F) test. It was observed that there was no significant difference between these methods. These two methods were then evaluated using the AGREE-Analytical GREEnness metric software. The chromatographic method using ethanol as an organic modifier has been proposed as an excellent eco-friendly and analyst-friendly alternative for the determination of mirtazapine in pharmaceutical formulations.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"134975303","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}
Abstract It still remains a great challenge to selectively enrich and sensitively quantify the trace volatile organic compounds (VOCs) in real samples with complex matrix. In this study, an integration method combining a selective enrichment medium of reduced graphene oxide (rGO) with a specially designed micro thermal-assisted purge-and-trap sampling device was developed for efficient enrichment and sensitive quantification of trace tobacco VOCs coupling with thermal desorption (TD)-gas chromatography/mass spectrometry (GC/MS). The prepared rGO has been proved to possess excellent enrichment selectivity and capacity for tobacco polar VOCs with the multi-layer structure, good thermal stability and large specific surface area. The specially designed sampling device was efficient and suitable for enriching and sampling trace polar tobacco VOCs coupling with rGO medium. Under the optimized sampling and analytical conditions, the established analytical method could be actually applied for quantification of typical tobacco polar VOCs with the good recoveries of 72.9–128% and the satisfied RSDs of 1.8–19.9% ( n = 3). The results suggested that the developed method was selective, sensitive and reliable for enrichment and quantification of trace tobacco polar VOCs.
{"title":"Efficient and sensitive quantification of polar tobacco volatile organic compounds by a micro thermal-assisted sampling device using reduced graphene oxide coupling with thermal desorption-gas chromatography/mass spectrometry","authors":"Yanhua Lai, Bing Han, Jiahui Wu, Shouhui Weng, Senlin Chen, Junxia Wang, Yu Wang, Xiaowei Pan, Yun Lin, Hong Tao, Zhuomin Zhang, Gongke Li","doi":"10.1556/1326.2023.01161","DOIUrl":"https://doi.org/10.1556/1326.2023.01161","url":null,"abstract":"Abstract It still remains a great challenge to selectively enrich and sensitively quantify the trace volatile organic compounds (VOCs) in real samples with complex matrix. In this study, an integration method combining a selective enrichment medium of reduced graphene oxide (rGO) with a specially designed micro thermal-assisted purge-and-trap sampling device was developed for efficient enrichment and sensitive quantification of trace tobacco VOCs coupling with thermal desorption (TD)-gas chromatography/mass spectrometry (GC/MS). The prepared rGO has been proved to possess excellent enrichment selectivity and capacity for tobacco polar VOCs with the multi-layer structure, good thermal stability and large specific surface area. The specially designed sampling device was efficient and suitable for enriching and sampling trace polar tobacco VOCs coupling with rGO medium. Under the optimized sampling and analytical conditions, the established analytical method could be actually applied for quantification of typical tobacco polar VOCs with the good recoveries of 72.9–128% and the satisfied RSDs of 1.8–19.9% ( n = 3). The results suggested that the developed method was selective, sensitive and reliable for enrichment and quantification of trace tobacco polar VOCs.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135592263","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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