Acta Chromatographica最新文献

{"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}

{"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}

{"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}

{"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}

{"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}

{"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}

{"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}

{"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}

{"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}

{"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}