Shaileshkumar K. Koradia, Madhavi Patel, A. Sen, D. Sen, Prasanna Pradhan
The current study aims to develop and validate an analytical quality by design approach‐based high‐performance thin‐layer chromatographic (HPTLC) method for the analysis of Axitinib tablet samples. The chromatographic conditions in the TLC method were optimized using a three‐level full factorial design. The mobile phase composition and chamber saturation time served as the independent variables for optimization. The mobile phase used for TLC separation on pre‐coated aluminum plates with silica gel 60 F254 consisted of a mixture of ethyl acetate and isopropyl alcohol in a ratio of 9:1 (v/v). Axitinib was quantified at 330 nm using the densitometric method. Axitinib peak from tablet formulation was verified against the reference standard by comparing its single band at Rf 0.44 ± 0.02. Linearity was found to exist between 100 and 600 ng/band, with a correlation coefficient (r2) of 0.9978. The percentage recovery was obtained as 98.21%–99.05%. The system was validated by determining the parameters according to the guidelines of the International Council for Harmonization of Technical Conditions for Medical Products for Human Use. The proposed TLC method can be effectively applied to routine quality control of a pharmaceutical product.
{"title":"Analytical quality by design‐based thin‐layer chromatography method development and validation for assay and content uniformity testing of the anti‐neoplastic drug Axitinib in tablet formulation","authors":"Shaileshkumar K. Koradia, Madhavi Patel, A. Sen, D. Sen, Prasanna Pradhan","doi":"10.1002/sscp.202300176","DOIUrl":"https://doi.org/10.1002/sscp.202300176","url":null,"abstract":"The current study aims to develop and validate an analytical quality by design approach‐based high‐performance thin‐layer chromatographic (HPTLC) method for the analysis of Axitinib tablet samples. The chromatographic conditions in the TLC method were optimized using a three‐level full factorial design. The mobile phase composition and chamber saturation time served as the independent variables for optimization. The mobile phase used for TLC separation on pre‐coated aluminum plates with silica gel 60 F254 consisted of a mixture of ethyl acetate and isopropyl alcohol in a ratio of 9:1 (v/v). Axitinib was quantified at 330 nm using the densitometric method. Axitinib peak from tablet formulation was verified against the reference standard by comparing its single band at Rf 0.44 ± 0.02. Linearity was found to exist between 100 and 600 ng/band, with a correlation coefficient (r2) of 0.9978. The percentage recovery was obtained as 98.21%–99.05%. The system was validated by determining the parameters according to the guidelines of the International Council for Harmonization of Technical Conditions for Medical Products for Human Use. The proposed TLC method can be effectively applied to routine quality control of a pharmaceutical product.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"41 1","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-12-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139005643","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}
Bereket Tesfaye, A. Gure, Tsegaye Girma Asere, Toleshi Teshome, Yerosan Buzayo
An efficient analytical method has been developed based on dispersive solid‐phase extraction followed by gas chromatography‐mass spectrometry for the determinations of 13 organochlorine pesticides in fruit juice samples. In this method, dispersive solid phase extraction was used for the extraction of target analye using iron‐doped zinc oxide nanoparticles supported with silica as a sorbent. Different experimental parameters affecting the extraction efficiencies the proposed method were carefully optimized. Under the optimum conditions, the calibration graphs were linear in the concentration range of 0.6–100 ng/mL with coefficients of determinations in the range of 0.9927–0.9991. The limits of detection and quantification determined as 3 and 10 times the signal‐to‐noise ratio were in the range of 0.01–0.03 and 0.6–1.0 ng/mL, respectively. Intra‐ and inter‐day precision studies of the proposed method, expressed as relative standard deviations, were in the range of 2.1%–9.2% and 2.2%–9.7%, respectively. The recoveries of the spiked fruit juices samples were in the range of 81.4%–105.1% with the corresponding relative standard deviations ranging from 1.0%–8.8%. In general, the proposed method demonstrated satisfactory analytical performance. Thus,it could be used as simple and attracive alternative method for the extraction of organochlorine pesticides from fruit juice sample and other related matrices.
{"title":"Dispersive solid‐phase extraction for the determination of organochlorine pesticides in fruit juice samples using iron‐doped zinc oxide nanoparticles supported with silica as a sorbent","authors":"Bereket Tesfaye, A. Gure, Tsegaye Girma Asere, Toleshi Teshome, Yerosan Buzayo","doi":"10.1002/sscp.202300161","DOIUrl":"https://doi.org/10.1002/sscp.202300161","url":null,"abstract":"An efficient analytical method has been developed based on dispersive solid‐phase extraction followed by gas chromatography‐mass spectrometry for the determinations of 13 organochlorine pesticides in fruit juice samples. In this method, dispersive solid phase extraction was used for the extraction of target analye using iron‐doped zinc oxide nanoparticles supported with silica as a sorbent. Different experimental parameters affecting the extraction efficiencies the proposed method were carefully optimized. Under the optimum conditions, the calibration graphs were linear in the concentration range of 0.6–100 ng/mL with coefficients of determinations in the range of 0.9927–0.9991. The limits of detection and quantification determined as 3 and 10 times the signal‐to‐noise ratio were in the range of 0.01–0.03 and 0.6–1.0 ng/mL, respectively. Intra‐ and inter‐day precision studies of the proposed method, expressed as relative standard deviations, were in the range of 2.1%–9.2% and 2.2%–9.7%, respectively. The recoveries of the spiked fruit juices samples were in the range of 81.4%–105.1% with the corresponding relative standard deviations ranging from 1.0%–8.8%. In general, the proposed method demonstrated satisfactory analytical performance. Thus,it could be used as simple and attracive alternative method for the extraction of organochlorine pesticides from fruit juice sample and other related matrices.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"7 1","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138982252","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}
Here, we deployed sol‐gel universal sorbent‐coated fabric phase sorptive extraction membranes in tandem with high‐performance liquid chromatography equipped with an ultraviolet detector (HPLC‐UV) for the analysis of 10 endocrine‐disrupting chemicals (EDCs). Due to the varying polarities of the studied compounds indicated by their octanol/water partition coefficient ‘log Kow’ (1.47–5.07), the extraction membrane was designed with different functionalities that are capable of simultaneous interaction with compounds of diverse natures including polar, non‐polar, and ionic species via sol‐gel sorbent coating technology. An isocratic mode of HPLC‐UV at 55:45% acetonitrile:water (v/v) on a reverse phase C18 Zorbax column (5 μm, 150 mm, 4.6 mm) was used for the separation and quantitation. Calibration curves were found linear between 25 and 2000 ppb for all compounds except cortisone in the range of 25–1000 ppb which provided an R2 value above 0.9940 in all cases. The intra‐day reproducibility and inter‐day reproducibility were found in the range of 1.2–12.8 and 0.2–14.1 (expressed as percent relative standard deviation), respectively. The validated method was finally deployed for the analysis of environmental water and milk samples with estradiol showing the highest concentrations among the studied compounds.
{"title":"Application of sol‐gel universal sorbent coated fabric phase sorptive extraction membranes in combination with high‐performance liquid chromatography‐ultraviolet detection to monitor endocrine‐disrupting chemicals in milk and environmental water samples","authors":"Basit Olayanju, A. Kabir, N. Manousi, K. Furton","doi":"10.1002/sscp.202300101","DOIUrl":"https://doi.org/10.1002/sscp.202300101","url":null,"abstract":"Here, we deployed sol‐gel universal sorbent‐coated fabric phase sorptive extraction membranes in tandem with high‐performance liquid chromatography equipped with an ultraviolet detector (HPLC‐UV) for the analysis of 10 endocrine‐disrupting chemicals (EDCs). Due to the varying polarities of the studied compounds indicated by their octanol/water partition coefficient ‘log Kow’ (1.47–5.07), the extraction membrane was designed with different functionalities that are capable of simultaneous interaction with compounds of diverse natures including polar, non‐polar, and ionic species via sol‐gel sorbent coating technology. An isocratic mode of HPLC‐UV at 55:45% acetonitrile:water (v/v) on a reverse phase C18 Zorbax column (5 μm, 150 mm, 4.6 mm) was used for the separation and quantitation. Calibration curves were found linear between 25 and 2000 ppb for all compounds except cortisone in the range of 25–1000 ppb which provided an R2 value above 0.9940 in all cases. The intra‐day reproducibility and inter‐day reproducibility were found in the range of 1.2–12.8 and 0.2–14.1 (expressed as percent relative standard deviation), respectively. The validated method was finally deployed for the analysis of environmental water and milk samples with estradiol showing the highest concentrations among the studied compounds.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"48 43","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-12-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138588630","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}
T. P. S. Laasya, S. Thapliyal, K. Goel, Bhupinder Kumar, Ramarao Poduri, Gaurav Joshi
An Indian traditional medicinal plant, Boerhaavia diffusa (Punarnava), is reported for its diuretic activity and helps in impaired kidney function. The present study indicates that alkaloids, carbohydrates, saponins, phytosterols, flavonoids, and glycosides are absent in the petroleum ether extract and present chiefly in the methanolic extract of roots. The phytosterols were found to be present in the ethyl acetate extract, while other phytochemical constituents, that is, alkaloids, carbohydrates, saponins, flavonoids, and glycosides, were absent. From high‐performance thin‐layer chromatography, the results indicated that out of all the three extracts and two marketed formulations, ethyl acetate root extract (LEA) has the highest amount of Boeravinone B content. Further, different root extracts of B. diffusa and two marketed formulations were evaluated on the human embryonic kidney cell line to understand pharmacological safety. From the results, it was observed that LEA and petroleum ether root extracts showed a higher percentage of cell survival and a better safety profile up to the dose of 1 mg/mL. The overall results indicated that further preclinical evaluation of B. diffusa is needed to understand the mechanism behind nephroprotective potential which can further expedite the drug discovery process of nephroprotective molecules.
{"title":"Phytochemical analysis and high‐performance thin‐layer chromatography guided quantification of Boeravinone B from Boerhaavia diffusa root extracts: Assessment of in vitro safety analysis","authors":"T. P. S. Laasya, S. Thapliyal, K. Goel, Bhupinder Kumar, Ramarao Poduri, Gaurav Joshi","doi":"10.1002/sscp.202300140","DOIUrl":"https://doi.org/10.1002/sscp.202300140","url":null,"abstract":"An Indian traditional medicinal plant, Boerhaavia diffusa (Punarnava), is reported for its diuretic activity and helps in impaired kidney function. The present study indicates that alkaloids, carbohydrates, saponins, phytosterols, flavonoids, and glycosides are absent in the petroleum ether extract and present chiefly in the methanolic extract of roots. The phytosterols were found to be present in the ethyl acetate extract, while other phytochemical constituents, that is, alkaloids, carbohydrates, saponins, flavonoids, and glycosides, were absent. From high‐performance thin‐layer chromatography, the results indicated that out of all the three extracts and two marketed formulations, ethyl acetate root extract (LEA) has the highest amount of Boeravinone B content. Further, different root extracts of B. diffusa and two marketed formulations were evaluated on the human embryonic kidney cell line to understand pharmacological safety. From the results, it was observed that LEA and petroleum ether root extracts showed a higher percentage of cell survival and a better safety profile up to the dose of 1 mg/mL. The overall results indicated that further preclinical evaluation of B. diffusa is needed to understand the mechanism behind nephroprotective potential which can further expedite the drug discovery process of nephroprotective molecules.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"33 4","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-12-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138592448","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}
Shikha Shah, C. Kothari, Krishna Bhalodi, Misari Patel
Diroximel fumarate (DRF) is a novel oral fumarate used in the treatment of multiple sclerosis. Comprehending DRF's stability behavior in different degradation conditions is crucial and has been studied under photolysis, oxidative, hydrolysis, and thermal conditions. Nucleosil C18 column (250 × 4.6 mm, 5 μm) was employed to achieve drug separation, with a mobile phase comprising of water and acetonitrile (65:35, v/v). The flow rate was 1 mL/min and detection was performed at 210 nm using a photodiode array detector. The fully validated reversed phase‐high‐performance liquid chromatography stability method as per the International Council for Harmonization Q2 R1 demonstrated excellent selectivity, accuracy, and precision with good sensitivity. During the analysis, two prominent degradant product peaks of DRF were identified across all stress conditions. The usage of liquid chromatography‐mass spectrometry compatible solvents in the mobile phase permits further characterization of DRF and its degradants peak. Significant levels of degradation were found in alkaline and acidic hydroxide, peroxide, photolytic, and thermal conditions with hydrolysis being postulated as a possible mechanism of degradation. The fully validated stability‐indicating analytical method can be used for routine quality control and stability testing of DRF, requiring storage in a protected primary container, as it is sensitive to light and moisture.
富马酸地洛昔梅尔(DRF)是一种用于治疗多发性硬化症的新型口服富马酸。了解DRF在不同降解条件下的稳定性行为至关重要，并在光解、氧化、水解和热条件下进行了研究。采用核sil C18色谱柱(250 × 4.6 mm, 5 μm)进行药物分离，流动相为水和乙腈(65:35,v/v)。流速为1 mL/min，使用光电二极管阵列检测器在210 nm处进行检测。根据国际统一理事会Q2 R1，完全验证的反相高效液相色谱稳定性方法具有良好的选择性、准确性和精密度，具有良好的灵敏度。在分析过程中，在所有应力条件下都确定了两个突出的DRF降解产物峰。在流动相中使用液相色谱-质谱相容溶剂可以进一步表征DRF及其降解物峰。在碱性和酸性氢氧化物、过氧化氢、光解和热条件下发现了显著的降解水平，水解被认为是降解的可能机制。完全验证的稳定性指示分析方法可用于DRF的常规质量控制和稳定性测试，因为它对光和水分敏感，需要储存在一个受保护的主容器中。
{"title":"A novel stability indicating mass compatible reversed‐phase high‐performance liquid chromatography for the determination of Diroximel fumarate and its related impurities","authors":"Shikha Shah, C. Kothari, Krishna Bhalodi, Misari Patel","doi":"10.1002/sscp.202300171","DOIUrl":"https://doi.org/10.1002/sscp.202300171","url":null,"abstract":"Diroximel fumarate (DRF) is a novel oral fumarate used in the treatment of multiple sclerosis. Comprehending DRF's stability behavior in different degradation conditions is crucial and has been studied under photolysis, oxidative, hydrolysis, and thermal conditions. Nucleosil C18 column (250 × 4.6 mm, 5 μm) was employed to achieve drug separation, with a mobile phase comprising of water and acetonitrile (65:35, v/v). The flow rate was 1 mL/min and detection was performed at 210 nm using a photodiode array detector. The fully validated reversed phase‐high‐performance liquid chromatography stability method as per the International Council for Harmonization Q2 R1 demonstrated excellent selectivity, accuracy, and precision with good sensitivity. During the analysis, two prominent degradant product peaks of DRF were identified across all stress conditions. The usage of liquid chromatography‐mass spectrometry compatible solvents in the mobile phase permits further characterization of DRF and its degradants peak. Significant levels of degradation were found in alkaline and acidic hydroxide, peroxide, photolytic, and thermal conditions with hydrolysis being postulated as a possible mechanism of degradation. The fully validated stability‐indicating analytical method can be used for routine quality control and stability testing of DRF, requiring storage in a protected primary container, as it is sensitive to light and moisture.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"11 3","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-12-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138592695","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}
Tinku Gupta, NaliniKanta Sahoo, Maddela Rambabu, M. Praveen, Shrikant Charde, Madhusmita Sahu, Prasun Chakrabarti, Bui Thanh Hung, Martin Margala, B. Unhelkar, A. Narayanankutty
Dacomitinib, a quinazoline compound, exhibits antineoplastic activity against brain metastasis activities in non‐small cell lung cancer and the central nervous system. In this study, the liquid–liquid extraction method with high‐performance liquid chromatography and tandem mass spectrometry detection method was established and validated for the determination of Dacomitinib in human plasma. Plasma samples were prepared and chromatographic separation was achieved on analytical column Discovery C18 (10 cm × 4.6 mm, 5 μm) with gradient elutes at a flow rate of 0.8 mL/min, using a mobile phase consisting of acetonitrile and ammonium formate. Dacomitinib and dacomitinib D10 (internal standard) were detected by multiple reactions. The method was fully validated according to the United States Food and Drug Administration guidelines. The calibration curve was linear with an excellent correlation coefficient (r2 ˂ 0.99). The method validation steps such as carry‐over, matrix effect, extraction recovery, dilution effect, intra‐inter accuracy, and precision were found within acceptable limits. The method was then applied to a pharmacokinetic study in human plasma. After oral administration, the plasma concentration in different volunteers reached 0.5–250.01 ng/mL. The result established can be applied to the estimation of drugs in human plasma.
Dacomitinib是一种喹唑啉类化合物，在非小细胞肺癌和中枢神经系统中表现出抗脑转移活性。本研究建立了高效液相色谱-串联质谱法的液液萃取法，并对测定人血浆中达科米替尼的方法进行了验证。制备血浆样品，采用梯度洗脱柱Discovery C18 (10 cm × 4.6 mm, 5 μm)，流速为0.8 mL/min，流动相为乙腈-甲酸铵，进行色谱分离。采用多反应法检测达科替尼和达科替尼D10(内标)。根据美国食品和药物管理局的指导方针，该方法得到了充分验证。标定曲线呈良好的线性关系(r2小于0.99)。方法验证步骤如携带、基质效应、萃取回收率、稀释效应、内部准确度和精密度均在可接受范围内。然后将该方法应用于人血浆药代动力学研究。口服给药后，不同志愿者血药浓度均达到0.5 ~ 250.01 ng/mL。所建立的结果可用于人血浆中药物含量的估计。
{"title":"New validated liquid chromatography‐tandem mass spectrometry method for the determination of Dacomitinib in human plasma and its application to a pharmacokinetic study","authors":"Tinku Gupta, NaliniKanta Sahoo, Maddela Rambabu, M. Praveen, Shrikant Charde, Madhusmita Sahu, Prasun Chakrabarti, Bui Thanh Hung, Martin Margala, B. Unhelkar, A. Narayanankutty","doi":"10.1002/sscp.202300131","DOIUrl":"https://doi.org/10.1002/sscp.202300131","url":null,"abstract":"Dacomitinib, a quinazoline compound, exhibits antineoplastic activity against brain metastasis activities in non‐small cell lung cancer and the central nervous system. In this study, the liquid–liquid extraction method with high‐performance liquid chromatography and tandem mass spectrometry detection method was established and validated for the determination of Dacomitinib in human plasma. Plasma samples were prepared and chromatographic separation was achieved on analytical column Discovery C18 (10 cm × 4.6 mm, 5 μm) with gradient elutes at a flow rate of 0.8 mL/min, using a mobile phase consisting of acetonitrile and ammonium formate. Dacomitinib and dacomitinib D10 (internal standard) were detected by multiple reactions. The method was fully validated according to the United States Food and Drug Administration guidelines. The calibration curve was linear with an excellent correlation coefficient (r2 ˂ 0.99). The method validation steps such as carry‐over, matrix effect, extraction recovery, dilution effect, intra‐inter accuracy, and precision were found within acceptable limits. The method was then applied to a pharmacokinetic study in human plasma. After oral administration, the plasma concentration in different volunteers reached 0.5–250.01 ng/mL. The result established can be applied to the estimation of drugs in human plasma.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"87 3","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-12-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138590804","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}
People's health benefits from andrographolide (ANDRO), apigenin (API), gallic acid (GA), and apocynin (APO) because they aid in the treatment of liver illness. The study mainly illustrated that a green approach is essential in the medical sector as well as the herbal sector with the help of “Green Analytical quality by design”. The mobile phase combination Dichloromethane: Ethyl acetate: Formic acid (10:8:0.4)v/v/v was optimized with the aid of an analytical quality‐by‐design approach. The absorbance mode at 254 nm was chosen for densitometric analysis as it gives a compact spot of ANDRO, API, GA, and APO at RF values of 0.24, 0.55, 0.17, and 0.68. Linearity was obtained in the range of 200–800 ng for all four markers. After retardation factor, ANDRO, APO, API, and GA from the tablet were found 0.0433, 0.0020, 0.1356, and 0.0015 mg, respectively. The validation parameter of R2 value ranged from 0.998, 0.999, 0.996, and 0.998 for all four ANDRO, API, GA, and APO. The study's findings revealed that the “high‐performance thin layer chromatography” technology is an environmentally friendly analytical design that helps to maintain the stability of the medication. It was also acknowledged as a quality design and a fresh idea in the pharmaceutical industry.
{"title":"Simultaneous estimation of andrographolide, apigenin, apocynin, and gallic acid by high‐performance thin layer chromatography method with Greenness quality by design approach","authors":"Shweta Mevada, Saurabh Shukla, Harsha Patel","doi":"10.1002/sscp.202300109","DOIUrl":"https://doi.org/10.1002/sscp.202300109","url":null,"abstract":"People's health benefits from andrographolide (ANDRO), apigenin (API), gallic acid (GA), and apocynin (APO) because they aid in the treatment of liver illness. The study mainly illustrated that a green approach is essential in the medical sector as well as the herbal sector with the help of “Green Analytical quality by design”. The mobile phase combination Dichloromethane: Ethyl acetate: Formic acid (10:8:0.4)v/v/v was optimized with the aid of an analytical quality‐by‐design approach. The absorbance mode at 254 nm was chosen for densitometric analysis as it gives a compact spot of ANDRO, API, GA, and APO at RF values of 0.24, 0.55, 0.17, and 0.68. Linearity was obtained in the range of 200–800 ng for all four markers. After retardation factor, ANDRO, APO, API, and GA from the tablet were found 0.0433, 0.0020, 0.1356, and 0.0015 mg, respectively. The validation parameter of R2 value ranged from 0.998, 0.999, 0.996, and 0.998 for all four ANDRO, API, GA, and APO. The study's findings revealed that the “high‐performance thin layer chromatography” technology is an environmentally friendly analytical design that helps to maintain the stability of the medication. It was also acknowledged as a quality design and a fresh idea in the pharmaceutical industry.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"25 12","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-12-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138591229","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}
M. Farajzadeh, Ali Hoboobi, S. Pezhhanfar, M. Mogaddam
In this study, a swift and economical extraction and preconcentration method called effervescence‐assisted dispersive liquid‐phase microextraction was developed to analyze the pesticide content of different grape juices. To propel the microextraction method, the sample was transferred to a conical bottom glass test tube, and ammonium chloride was added and vortexed to dissolve. Then, sodium bicarbonate and a mixture of 1,2‐dibromoethane and n‐hexane were added. The tube was located in a water bath and the produced carbon dioxide bubbles dispersed the extraction solvent into the sample. Finally, it was centrifuged and one microliter of the sedimented phase was injected into a gas chromatograph equipped with a flame ionization detector. Under the optimum conditions, the limits of detection and quantification ranged from 0.9 to 4.1 and 3.0 to 13.6 μg/L, respectively. Extraction recoveries and enrichment factors were achieved in the ranges of 36%–80% and 180%–404%, respectively. The inter‐ and intra‐day relative standard deviations were in the ranges of 3.4%–10.6% and 2.6%–9.7%, respectively. Also, the coefficients of determination in the calibration curves were ≥0.990. Short extraction time, no sorbent or costly apparatuses, using inexpensive chemicals, applying microliter levels of the extractant, and no dilution of the real samples are the highlights of the study.
{"title":"Development of an effervescence‐assisted dispersive liquid phase microextraction using a binary solvent as a simultaneous extraction and preconcentration approach specialized for the analysis of pesticides in grape juice without dilution","authors":"M. Farajzadeh, Ali Hoboobi, S. Pezhhanfar, M. Mogaddam","doi":"10.1002/sscp.202300195","DOIUrl":"https://doi.org/10.1002/sscp.202300195","url":null,"abstract":"In this study, a swift and economical extraction and preconcentration method called effervescence‐assisted dispersive liquid‐phase microextraction was developed to analyze the pesticide content of different grape juices. To propel the microextraction method, the sample was transferred to a conical bottom glass test tube, and ammonium chloride was added and vortexed to dissolve. Then, sodium bicarbonate and a mixture of 1,2‐dibromoethane and n‐hexane were added. The tube was located in a water bath and the produced carbon dioxide bubbles dispersed the extraction solvent into the sample. Finally, it was centrifuged and one microliter of the sedimented phase was injected into a gas chromatograph equipped with a flame ionization detector. Under the optimum conditions, the limits of detection and quantification ranged from 0.9 to 4.1 and 3.0 to 13.6 μg/L, respectively. Extraction recoveries and enrichment factors were achieved in the ranges of 36%–80% and 180%–404%, respectively. The inter‐ and intra‐day relative standard deviations were in the ranges of 3.4%–10.6% and 2.6%–9.7%, respectively. Also, the coefficients of determination in the calibration curves were ≥0.990. Short extraction time, no sorbent or costly apparatuses, using inexpensive chemicals, applying microliter levels of the extractant, and no dilution of the real samples are the highlights of the study.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"13 24","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-12-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"138602153","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}
Yumei Wang, Meiling Gu, Jialin Mao, Jianhua Liu, Songjie Fan, Honglian Zhang, Hongzhou Bu, Qi Liu
Flavonoid‐C‐glycosides with various pharmacological actions were abundant in corn silk, and fragmentation in mass spectra of flavonoid‐C‐glycosides compounds was particularly important. This paper aimed to supervise the fragmentation patterns of flavonoid‐C‐glycosides in the enriched flavonoids from corn silk by high‐efficiency ultra‐high‐performance liquid chromatography combined with a quadrupole time‐of‐flight mass spectrometry approach. Therefore, the flavonoids were extracted by heating reflux and then purified based on D101 macroporous resin. Thirty‐five flavonoids were triumphantly identified in the purified product. Among them, 14 were flavonoid‐C‐glycosides, seven of them owned luteolin mother nuclei (luteolin‐C‐glycosides) and seven of them owned apigenin mother nuclei (apigenin‐C‐glycosides). Importantly, the diagnostic product ions of luteolin‐C‐glycosides including m/z (431, 413, 395, 369, 367, 313, and 299) and m/z (429, 411, 393, 367, 365, 311, and 297), and the characteristic product ions of apigenin‐C‐glycosides covered m/z (353, 339, and 299) and m/z (339, 327, and 309). In addition, diagnostic H2O neutral loss and glycosyl craking were familiar, and the difference values among product ions mainly contained 40, 60, 70, 80, 90, 100, and 120 Da. Thus, the fragmentations of luteolin‐C‐glycosides and apigenin‐C‐glycosides identified in corn silk were with proper regularity. The obtained fragmentation patterns provided rapid recognition and meaningful guidance for the purification study of flavonoid‐C‐glycosides.
{"title":"Phytochemical study: Fragmentation patterns of flavonoid‐C‐glycosides in the enriched flavonoids from corn silk using high‐efficiency ultra‐high‐performance liquid chromatography combined with quadrupole time‐of‐flight mass spectrometry","authors":"Yumei Wang, Meiling Gu, Jialin Mao, Jianhua Liu, Songjie Fan, Honglian Zhang, Hongzhou Bu, Qi Liu","doi":"10.1002/sscp.202300156","DOIUrl":"https://doi.org/10.1002/sscp.202300156","url":null,"abstract":"Flavonoid‐C‐glycosides with various pharmacological actions were abundant in corn silk, and fragmentation in mass spectra of flavonoid‐C‐glycosides compounds was particularly important. This paper aimed to supervise the fragmentation patterns of flavonoid‐C‐glycosides in the enriched flavonoids from corn silk by high‐efficiency ultra‐high‐performance liquid chromatography combined with a quadrupole time‐of‐flight mass spectrometry approach. Therefore, the flavonoids were extracted by heating reflux and then purified based on D101 macroporous resin. Thirty‐five flavonoids were triumphantly identified in the purified product. Among them, 14 were flavonoid‐C‐glycosides, seven of them owned luteolin mother nuclei (luteolin‐C‐glycosides) and seven of them owned apigenin mother nuclei (apigenin‐C‐glycosides). Importantly, the diagnostic product ions of luteolin‐C‐glycosides including m/z (431, 413, 395, 369, 367, 313, and 299) and m/z (429, 411, 393, 367, 365, 311, and 297), and the characteristic product ions of apigenin‐C‐glycosides covered m/z (353, 339, and 299) and m/z (339, 327, and 309). In addition, diagnostic H2O neutral loss and glycosyl craking were familiar, and the difference values among product ions mainly contained 40, 60, 70, 80, 90, 100, and 120 Da. Thus, the fragmentations of luteolin‐C‐glycosides and apigenin‐C‐glycosides identified in corn silk were with proper regularity. The obtained fragmentation patterns provided rapid recognition and meaningful guidance for the purification study of flavonoid‐C‐glycosides.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"20 S1","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-11-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139247380","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}
Zhengming Qian, Jing Chen, Qing-Qing Lei, Guoying Tan, Yuansheng Zou, Gang Peng, Juying Xie, Wenqing Li
Herbal medicine is a complex system containing numerous bioactive components. Evaluating the quality of herbs often requires analyzing multiple components using high‐performance liquid chromatography (HPLC). However, existing HPLC methods are time‐consuming and consume large amounts of reference compounds. This study, an ultra‐rapid and green assay method for the determination of honokiol and magnolol in Magnoliae Officinalis Cortex using a single reference compound was developed by HPLC at equal absorption wavelength (EAW). The sample was prepared using ultrasonic‐assisted matrix solid‐phase dispersion and separated with an eco‐friendly mobile phase on the Poroshell C18 column. The EAW of homokiol and magnolol was chosen as the detecting wavelength (247 nm). The contents of honokiol and magnolol in six Magnoliae Officinalis Cortex samples obtained by the developed method with a single marker and the external standard method with two markers were comparable. Additionally, the developed HPLC process only needed 4.55 mL green organic solution (ethanol) and 2.5 min, which included sample extraction and separation. The developed HPLC EAW method was ultra‐fast, green, and reference compound saving, which was an improved quality control method of Magnoliae Officinalis Cortex and would serve as an example for the determination of multiple components in other herbal medicines using a single reference compound.
{"title":"Rapid determination of multiple components in herbal medicine using a single reference compound by high‐performance liquid chromatography at equal absorption wavelength: Case study of Magnoliae officinalis cortex","authors":"Zhengming Qian, Jing Chen, Qing-Qing Lei, Guoying Tan, Yuansheng Zou, Gang Peng, Juying Xie, Wenqing Li","doi":"10.1002/sscp.202300071","DOIUrl":"https://doi.org/10.1002/sscp.202300071","url":null,"abstract":"Herbal medicine is a complex system containing numerous bioactive components. Evaluating the quality of herbs often requires analyzing multiple components using high‐performance liquid chromatography (HPLC). However, existing HPLC methods are time‐consuming and consume large amounts of reference compounds. This study, an ultra‐rapid and green assay method for the determination of honokiol and magnolol in Magnoliae Officinalis Cortex using a single reference compound was developed by HPLC at equal absorption wavelength (EAW). The sample was prepared using ultrasonic‐assisted matrix solid‐phase dispersion and separated with an eco‐friendly mobile phase on the Poroshell C18 column. The EAW of homokiol and magnolol was chosen as the detecting wavelength (247 nm). The contents of honokiol and magnolol in six Magnoliae Officinalis Cortex samples obtained by the developed method with a single marker and the external standard method with two markers were comparable. Additionally, the developed HPLC process only needed 4.55 mL green organic solution (ethanol) and 2.5 min, which included sample extraction and separation. The developed HPLC EAW method was ultra‐fast, green, and reference compound saving, which was an improved quality control method of Magnoliae Officinalis Cortex and would serve as an example for the determination of multiple components in other herbal medicines using a single reference compound.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":"159 3","pages":""},"PeriodicalIF":1.1,"publicationDate":"2023-11-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139258482","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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