Pub Date : 2023-05-04DOI: 10.1080/22297928.2023.2244492
B. Gowramma, S. Ramachandran, Kaviarasan Lakshmanan, R. Kalirajan, S. N. Meyyanathan, G. Swaminathan
Abstract The aim of this study was to develop a simple, specific, sensitive and precise LC-MS method for the determination of mebeverine enantiomers in pharmaceutical formulations and it was validated as per ICH guidelines. The chromatographic separation was achieved on Phenomenex® Lux Cellulose 1 (250 mm x 4.6 mm i.d, 5μm particle size) column using mobile phase system containing acetonitrile: 10 mM ammonium acetate (85:15) at the flow rate of 0.8 mL/min. In the spectral investigation by LC-MS, the standard solution of Mebeverine showed major peak at m/z of 430.70, which was assigned to the [M+H] ion of Mebeverine. The described method was linear over the range of 15–75 ng /mL for (±) Mebeverine enantiomers with a correlation coefficient (r2 = 0.999). Detection limits and quantification limits of (+) Mebeverine and (-) Mebeverine were found to be 5 ng/mL and 15 ng/mL respectively. The recovery study of mebeverine from tablet formulation was found to be 99.16%. Mebeverine standard solution and mobile phase were found to be stable for at least 48h. The Mebeverine enantiomers were well resolved with mean retention times of about 1.16 min and 1.20 min respectively. The developed method was extensively validated and proved to be robust, accurate, precise, and suitable for analysis of Mebeverine enantiomers in tablet dosage form. GRAPHICAL ABSTRACT
摘要:本研究旨在建立一种简便、特异、灵敏、精确的液相色谱-质谱法测定制剂中美贝弗林对映体的方法，并按照ICH指南进行验证。色谱柱为Phenomenex®Lux Cellulose 1 (250 mm × 4.6 mm i.d, 5μm粒径)，流动相为乙腈:10 mm醋酸铵(85:15)，流速为0.8 mL/min。在LC-MS谱分析中，Mebeverine标准溶液在m/z为430.70处出现主峰，归属于Mebeverine的[m +H]离子。Mebeverine对映体(±)在15 ~ 75 ng /mL范围内呈线性，相关系数(r2 = 0.999)。(+) Mebeverine的检出限为5 ng/mL， (-) Mebeverine的定量限为15 ng/mL。对片剂中美贝弗林的回收率进行了研究，回收率为99.16%。Mebeverine标准液和流动相稳定时间至少为48h。Mebeverine对映体分离效果良好，平均保留时间分别为1.16 min和1.20 min。结果表明，该方法可靠、准确、精密度高，适用于片剂型美贝弗林对映体的分析。图形抽象
{"title":"Development and validation of a chiral LC-MS method for the enantiomeric resolution of (+) and (-)-Mebeverine Hydrochloride in bulk drug by using polysaccharide-based chiral stationary phase","authors":"B. Gowramma, S. Ramachandran, Kaviarasan Lakshmanan, R. Kalirajan, S. N. Meyyanathan, G. Swaminathan","doi":"10.1080/22297928.2023.2244492","DOIUrl":"https://doi.org/10.1080/22297928.2023.2244492","url":null,"abstract":"Abstract The aim of this study was to develop a simple, specific, sensitive and precise LC-MS method for the determination of mebeverine enantiomers in pharmaceutical formulations and it was validated as per ICH guidelines. The chromatographic separation was achieved on Phenomenex® Lux Cellulose 1 (250 mm x 4.6 mm i.d, 5μm particle size) column using mobile phase system containing acetonitrile: 10 mM ammonium acetate (85:15) at the flow rate of 0.8 mL/min. In the spectral investigation by LC-MS, the standard solution of Mebeverine showed major peak at m/z of 430.70, which was assigned to the [M+H] ion of Mebeverine. The described method was linear over the range of 15–75 ng /mL for (±) Mebeverine enantiomers with a correlation coefficient (r2 = 0.999). Detection limits and quantification limits of (+) Mebeverine and (-) Mebeverine were found to be 5 ng/mL and 15 ng/mL respectively. The recovery study of mebeverine from tablet formulation was found to be 99.16%. Mebeverine standard solution and mobile phase were found to be stable for at least 48h. The Mebeverine enantiomers were well resolved with mean retention times of about 1.16 min and 1.20 min respectively. The developed method was extensively validated and proved to be robust, accurate, precise, and suitable for analysis of Mebeverine enantiomers in tablet dosage form. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"5 1","pages":"313 - 320"},"PeriodicalIF":0.0,"publicationDate":"2023-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75031554","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-04DOI: 10.1080/22297928.2023.2232786
Tahirah Khaliq, Sadaqat Farooq, M. Waseem, P. Sultan, Sabiyah Akhter, Q. P. Hassan
Abstract Rumex dentatus is traditionally used to treat different ailments including bacterial and fungal infections. The presented study disclosed isolation of five bioactive molecules from Rumex dentatus. All the isolates were evaluated for antimicrobial activities. In this protocol the comparative study has been made on various extracts and isolated compounds in order to identify the lead molecule. Thus the activity carried, resulted, compound X2 with strong anti-microbial potential and exhibiting IC50 value between 14–32 μM. While rest of isolates showed moderate antibacterial potential. Further, the investigation of antimicrobial activity on various plant extracts against six human pathogens (five bacteria and a fungal pathogen), most of the extracts showed strong to moderate antimicrobial activity with IC50 ranging from 24–35 μM. Out of all the extracts which were evaluated for antimicrobial activities, the hexane and methanol: DCM (1:1) extracts were found to have good antibacterial potential in microtiter plate assay. The IC50 value of compound X2 was found to be favorable and presented a strong antimicrobial potential. Thus the results inferred that the plant has strong antibacterial value and hence can be used in medication for the treatment of various bacterial infections. GRAPHICAL ABSTRACT
{"title":"Isolation of bioactive natural products from Rumex dentatus and their antimicrobial evaluation: A comparative study against various pathogenic bacteria","authors":"Tahirah Khaliq, Sadaqat Farooq, M. Waseem, P. Sultan, Sabiyah Akhter, Q. P. Hassan","doi":"10.1080/22297928.2023.2232786","DOIUrl":"https://doi.org/10.1080/22297928.2023.2232786","url":null,"abstract":"Abstract Rumex dentatus is traditionally used to treat different ailments including bacterial and fungal infections. The presented study disclosed isolation of five bioactive molecules from Rumex dentatus. All the isolates were evaluated for antimicrobial activities. In this protocol the comparative study has been made on various extracts and isolated compounds in order to identify the lead molecule. Thus the activity carried, resulted, compound X2 with strong anti-microbial potential and exhibiting IC50 value between 14–32 μM. While rest of isolates showed moderate antibacterial potential. Further, the investigation of antimicrobial activity on various plant extracts against six human pathogens (five bacteria and a fungal pathogen), most of the extracts showed strong to moderate antimicrobial activity with IC50 ranging from 24–35 μM. Out of all the extracts which were evaluated for antimicrobial activities, the hexane and methanol: DCM (1:1) extracts were found to have good antibacterial potential in microtiter plate assay. The IC50 value of compound X2 was found to be favorable and presented a strong antimicrobial potential. Thus the results inferred that the plant has strong antibacterial value and hence can be used in medication for the treatment of various bacterial infections. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"52 5 1","pages":"226 - 233"},"PeriodicalIF":0.0,"publicationDate":"2023-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77784290","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-04DOI: 10.1080/22297928.2023.2243279
Bhagavan Rajesh Babu Koppisetty, Hemant Kumar Tatapudi, Vasudha Dadi, Puthi Renuka Gayathri, P.N.Varalakshmi.K D. Komali, G. N. Challa, Varaprasada Rao Kollabathula, S. R. Yarraguntla
Abstract The current studies entail Quality by Design (QbD)-enabled development of a simple, rapid, sensitive and cost-effective high-performance liquid chromatographic method for estimation of emtricitabine (EMT), tenofovir diproxil fumarate (TEN), and efavirenz (EFA) in combined dosage form. Systematic optimization was performed employing Box-Behnken design by selecting the flow rate, buffer molarity, and acetonitrile volume as the critical method parameters (CMPs) identified from screening studies, thus evaluating the critical analytical attributes (CAAs), namely, retention duration, theoretical plates, resolution, and asymmetry factor as the parameters of method robustness. The optimal chromatographic separation was achieved using acetonitrile and phosphate buffer (pH 3.0) 74.1:25.9 v/v as the mobile phase with a flow rate 0.91 mL/min, and UV detection at 260 nm. The method was validated as per the ICH recommended conditions, which revealed high degree of linearity, accuracy, precision, sensitivity and robustness over the existing liquid chromatographic methods of the drug. Studies on forced degradation under acid, basic, oxidative, photolytic, and thermal conditions revealed the drug’s well-resolved peak and the degradation products’ peaks as well. GRAPHICAL ABSTRACT
{"title":"QbD based RP-HPLC method for simultaneous determination of a emtricitabine, tenofovir diproxil fumarate and efavirenz in tablet dosage form-an application to stability indicating assay","authors":"Bhagavan Rajesh Babu Koppisetty, Hemant Kumar Tatapudi, Vasudha Dadi, Puthi Renuka Gayathri, P.N.Varalakshmi.K D. Komali, G. N. Challa, Varaprasada Rao Kollabathula, S. R. Yarraguntla","doi":"10.1080/22297928.2023.2243279","DOIUrl":"https://doi.org/10.1080/22297928.2023.2243279","url":null,"abstract":"Abstract The current studies entail Quality by Design (QbD)-enabled development of a simple, rapid, sensitive and cost-effective high-performance liquid chromatographic method for estimation of emtricitabine (EMT), tenofovir diproxil fumarate (TEN), and efavirenz (EFA) in combined dosage form. Systematic optimization was performed employing Box-Behnken design by selecting the flow rate, buffer molarity, and acetonitrile volume as the critical method parameters (CMPs) identified from screening studies, thus evaluating the critical analytical attributes (CAAs), namely, retention duration, theoretical plates, resolution, and asymmetry factor as the parameters of method robustness. The optimal chromatographic separation was achieved using acetonitrile and phosphate buffer (pH 3.0) 74.1:25.9 v/v as the mobile phase with a flow rate 0.91 mL/min, and UV detection at 260 nm. The method was validated as per the ICH recommended conditions, which revealed high degree of linearity, accuracy, precision, sensitivity and robustness over the existing liquid chromatographic methods of the drug. Studies on forced degradation under acid, basic, oxidative, photolytic, and thermal conditions revealed the drug’s well-resolved peak and the degradation products’ peaks as well. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"1 1","pages":"267 - 288"},"PeriodicalIF":0.0,"publicationDate":"2023-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89771019","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-04DOI: 10.1080/22297928.2023.2242862
Sahena Ferdosh, Kashif Ghafoor, Md. Zaidul Islam Sarker
The date palm (Phoenix dactylifera L.) is one of the oldest fruit crops grown in the arid regions of the Arabian Peninsula, North Africa, and the Middle East. It has numerous uses in medicine, pharmacognosy, and even religion, making it more than just a valuable food source. The aim of the study is to assess the yield percentage, total phenolic content (TPC), phenolic compositions, and antioxidant activity of three P. dactylifera cultivars, namely, Khudori, Sabaka, and Nabtat Ali, using methanol and hexane as solvents for Soxhlet extraction. The antioxidant potential of the extract was evaluated based on total phenolic content, the 2,2, diphenyl-2-picryl-hydroxyl (DPPH) assay, and the ferric-reducing antioxidant power (FRAP) assay, whereas phenolic compounds were identified and quantified using HPLC. Methanolic extracts of various seed cultivars showed higher yield recovery and TPC than hexane extracts. Khudori seeds demonstrated the highest antioxidant capacities compared to the other cultivars, with 124.54 ± 2.89 mg GAE /100 g for TPC, 79.67 ± 4.53 percentage inhibition for DPPH, and 1.49 ± 0.53 mMTE/100g for FRAP. It shows the potential of the Khudori seed extracts as a good source of antioxidant nutraceutical food and useful drug development that can help with free radical-related diseases.
{"title":"Total phenolic content and antioxidant activity of date palm (<i>Phoenix dactylifera</i> L.) seed extracts using soxhlet method","authors":"Sahena Ferdosh, Kashif Ghafoor, Md. Zaidul Islam Sarker","doi":"10.1080/22297928.2023.2242862","DOIUrl":"https://doi.org/10.1080/22297928.2023.2242862","url":null,"abstract":"The date palm (Phoenix dactylifera L.) is one of the oldest fruit crops grown in the arid regions of the Arabian Peninsula, North Africa, and the Middle East. It has numerous uses in medicine, pharmacognosy, and even religion, making it more than just a valuable food source. The aim of the study is to assess the yield percentage, total phenolic content (TPC), phenolic compositions, and antioxidant activity of three P. dactylifera cultivars, namely, Khudori, Sabaka, and Nabtat Ali, using methanol and hexane as solvents for Soxhlet extraction. The antioxidant potential of the extract was evaluated based on total phenolic content, the 2,2, diphenyl-2-picryl-hydroxyl (DPPH) assay, and the ferric-reducing antioxidant power (FRAP) assay, whereas phenolic compounds were identified and quantified using HPLC. Methanolic extracts of various seed cultivars showed higher yield recovery and TPC than hexane extracts. Khudori seeds demonstrated the highest antioxidant capacities compared to the other cultivars, with 124.54 ± 2.89 mg GAE /100 g for TPC, 79.67 ± 4.53 percentage inhibition for DPPH, and 1.49 ± 0.53 mMTE/100g for FRAP. It shows the potential of the Khudori seed extracts as a good source of antioxidant nutraceutical food and useful drug development that can help with free radical-related diseases.","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"27 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2023-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"136375138","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-04DOI: 10.1080/22297928.2023.2193588
Moazzim Soudagar, Bhaskar Kurangi, H. B. Chethan Kumar, S. Chimagave, Umesh Patil, Shruti Kolambkar
Abstract Berberine has been shown to have therapeutic advantages in the management of different diseases. Due to its actions and therapeutic applications, in compliance with “The International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use”. (ICH) recommendations; a quick, precise and specific HPLC method was developed and validated. The chromatographic separation was carried out with Column C18 (4.6 mm X 250 mm), (5 microns) using 0.1% orthophosphoric acid: acetonitrile (60:40) as mobile phase, with a flow rate of 1 ml/min and at a wavelength of 349 nm. The developed method was also used for the estimation of berberine in various commercial preparations and also with formulated berberine-loaded cubosomal nano formulation according to ICH guidelines. Furthermore, forced degradation studies of berberine were investigated. The novel analytical technique was identified to be linear over the concentration ranging from 2 μg/ml to 14 μg/ml with R2 > 0.997. The method developed was accurate (with % recovery of 98.24% to 99.31%), precise (%RSD < 2.0%), and robust. The limit of quantification and limit of detection for berberine was found to be 0.064 μg/ml and 0.021 μg/ml respectively. In the presence of degradation products, the drug peak was obtained. The peaks for berberine were detected in the marketed formulations containing berberine and hence, the developed method could be applied to the estimation of berberine in berberine-containing formulations. GRAPHICAL ABSTRACT
{"title":"Development and validation of a simple stability-indicating HPLC method for the quantitation of berberine in pharmaceuticals, ayurvedic, homeopathic products and novel nanoformulation","authors":"Moazzim Soudagar, Bhaskar Kurangi, H. B. Chethan Kumar, S. Chimagave, Umesh Patil, Shruti Kolambkar","doi":"10.1080/22297928.2023.2193588","DOIUrl":"https://doi.org/10.1080/22297928.2023.2193588","url":null,"abstract":"Abstract Berberine has been shown to have therapeutic advantages in the management of different diseases. Due to its actions and therapeutic applications, in compliance with “The International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use”. (ICH) recommendations; a quick, precise and specific HPLC method was developed and validated. The chromatographic separation was carried out with Column C18 (4.6 mm X 250 mm), (5 microns) using 0.1% orthophosphoric acid: acetonitrile (60:40) as mobile phase, with a flow rate of 1 ml/min and at a wavelength of 349 nm. The developed method was also used for the estimation of berberine in various commercial preparations and also with formulated berberine-loaded cubosomal nano formulation according to ICH guidelines. Furthermore, forced degradation studies of berberine were investigated. The novel analytical technique was identified to be linear over the concentration ranging from 2 μg/ml to 14 μg/ml with R2 > 0.997. The method developed was accurate (with % recovery of 98.24% to 99.31%), precise (%RSD < 2.0%), and robust. The limit of quantification and limit of detection for berberine was found to be 0.064 μg/ml and 0.021 μg/ml respectively. In the presence of degradation products, the drug peak was obtained. The peaks for berberine were detected in the marketed formulations containing berberine and hence, the developed method could be applied to the estimation of berberine in berberine-containing formulations. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"53 1","pages":"244 - 256"},"PeriodicalIF":0.0,"publicationDate":"2023-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74761854","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-05-04DOI: 10.1080/22297928.2023.2243276
Hamzeh Alkhatib, F. Mohamed, Awis Sukarni Mohmad Sabere, Hazem Choukaife, A. Doolaanea
Abstract This study aimed to develop and validate an ultrasonication-aided UV-Vis spectroscopy method for quantifying black seed oil (BSO) in alginate beads. The method utilized sonication at 10% power rate for 120 seconds to stabilize the emulsion droplet size of 10 mL of the emulsion diluents derived from breaking BSO-alginate beads in phosphate buffer. Absorbance measurements were taken at 400 nm, which was found to be the optimal wavelength for measuring the absorbance of turbid emulsion diluents. The method showed excellent linearity between 0.8 - 5 mg/mL (R2 = 0.9977), with Limit of Detection (LOD) and Limit of Quantification (LOQ) values of 0.082 and 0.249 mg/mL, respectively. The method also exhibited good accuracy and precision, with recovery percentages ranging from 98.02 - 101.9% (RSD = 0.15 - 1.24%) and intra-day/inter-day precision with RSD less than 2%. These findings suggest that the ultrasonication-aided spectroscopy method is a quick, accurate, and precise way to quantify encapsulated oils and could be useful for oils analysis during R&D, In Process Quality Control (IPQC), and Quality Control (QC) tests, as well as in other applications such as industrial manufacturing and academic research. GRAPHICAL ABSTRACT
{"title":"Emulsification-assisted spectroscopic analysis of black seed oil in alginate beads: method development and validation","authors":"Hamzeh Alkhatib, F. Mohamed, Awis Sukarni Mohmad Sabere, Hazem Choukaife, A. Doolaanea","doi":"10.1080/22297928.2023.2243276","DOIUrl":"https://doi.org/10.1080/22297928.2023.2243276","url":null,"abstract":"Abstract This study aimed to develop and validate an ultrasonication-aided UV-Vis spectroscopy method for quantifying black seed oil (BSO) in alginate beads. The method utilized sonication at 10% power rate for 120 seconds to stabilize the emulsion droplet size of 10 mL of the emulsion diluents derived from breaking BSO-alginate beads in phosphate buffer. Absorbance measurements were taken at 400 nm, which was found to be the optimal wavelength for measuring the absorbance of turbid emulsion diluents. The method showed excellent linearity between 0.8 - 5 mg/mL (R2 = 0.9977), with Limit of Detection (LOD) and Limit of Quantification (LOQ) values of 0.082 and 0.249 mg/mL, respectively. The method also exhibited good accuracy and precision, with recovery percentages ranging from 98.02 - 101.9% (RSD = 0.15 - 1.24%) and intra-day/inter-day precision with RSD less than 2%. These findings suggest that the ultrasonication-aided spectroscopy method is a quick, accurate, and precise way to quantify encapsulated oils and could be useful for oils analysis during R&D, In Process Quality Control (IPQC), and Quality Control (QC) tests, as well as in other applications such as industrial manufacturing and academic research. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"117 1","pages":"234 - 243"},"PeriodicalIF":0.0,"publicationDate":"2023-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86466962","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-03-04DOI: 10.1080/22297928.2023.2213262
Vishal U. Mane, Bhaskar Kurangi, Neha Bhasagi, S. Patil, Moazzim Soudagar, Umesh Patil
Abstract Acyclovir has been shown to have therapeutic advantages in the management of different viral diseases. Owing to its tremendous and attractive therapeutic applications, a quick, precise, and specific HPLC method was developed and validated in compliance with ICH guidelines. The chromatographic separation was carried out with Column C18 (4.6mm X 250mm), (5 microns) by using 0.1% orthophosphoric acid (OPA) buffer: Methanol (55:45) as mobile phase, with a flow rate of 1 ml/min and at a wavelength of 253 nm. The novel analytical technique showed a peak of acyclovir at 2.4 min. The method was identified to be linear over the concentration ranging from 2 to 14 μg/ml. The method developed was accurate (with 98% recovery), precise, and robust. The developed method was also used for the estimation of acyclovir in various commercial formulations and acyclovir-loaded cubosomal nanoformulation. Furthermore, forced degradation studies for acyclovir were estimated under different stress conditions. In the presence of degradation products, the acyclovir peak was unaffected indicating the suitability of the developed method. Therefore, the developed method could be applied to the estimation of acyclovir in acyclovir-containing formulations. GRAPHICAL ABSTRACT
摘要阿昔洛韦已被证明在不同病毒性疾病的治疗中具有治疗优势。由于高效液相色谱的巨大和有吸引力的治疗应用，开发了一种快速、精确和特异性的高效液相色谱方法，并根据ICH指南进行了验证。色谱分离采用C18柱(4.6mm X 250mm)，(5微米)，流动相为0.1%正磷酸(OPA)缓冲液:甲醇(55:45)，流速为1 ml/min，波长为253 nm。在2 ~ 14 μg/ml的浓度范围内，无环鸟苷的含量在2.4 min达到峰值。该方法准确(回收率98%)、精密度高、稳健性好。该方法还可用于各种商业制剂和负载阿昔洛韦的立方体纳米制剂中阿昔洛韦的估计。此外，在不同的胁迫条件下，对阿昔洛韦进行了强制降解研究。在存在降解产物的情况下，无环鸟苷峰不受影响，表明所开发的方法的适用性。因此，该方法可用于含阿昔洛韦制剂中阿昔洛韦的含量估算。图形抽象
{"title":"Development and Validation of a Simple Stability-Indicating HPLC Method for the Quantitation of Acyclovir in Pharma-ceuticals and Novel Nanoformulation","authors":"Vishal U. Mane, Bhaskar Kurangi, Neha Bhasagi, S. Patil, Moazzim Soudagar, Umesh Patil","doi":"10.1080/22297928.2023.2213262","DOIUrl":"https://doi.org/10.1080/22297928.2023.2213262","url":null,"abstract":"Abstract Acyclovir has been shown to have therapeutic advantages in the management of different viral diseases. Owing to its tremendous and attractive therapeutic applications, a quick, precise, and specific HPLC method was developed and validated in compliance with ICH guidelines. The chromatographic separation was carried out with Column C18 (4.6mm X 250mm), (5 microns) by using 0.1% orthophosphoric acid (OPA) buffer: Methanol (55:45) as mobile phase, with a flow rate of 1 ml/min and at a wavelength of 253 nm. The novel analytical technique showed a peak of acyclovir at 2.4 min. The method was identified to be linear over the concentration ranging from 2 to 14 μg/ml. The method developed was accurate (with 98% recovery), precise, and robust. The developed method was also used for the estimation of acyclovir in various commercial formulations and acyclovir-loaded cubosomal nanoformulation. Furthermore, forced degradation studies for acyclovir were estimated under different stress conditions. In the presence of degradation products, the acyclovir peak was unaffected indicating the suitability of the developed method. Therefore, the developed method could be applied to the estimation of acyclovir in acyclovir-containing formulations. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"11 1","pages":"191 - 201"},"PeriodicalIF":0.0,"publicationDate":"2023-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84942862","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-03-04DOI: 10.1080/22297928.2023.2222281
A. Salem
Abstract Here, valuable elements in Talet Seleim, Southwestern Sinai, Egypt, were leached using methanesulfonic acid (MSA) as an environmentally friendly lixiviant agent. The effects of methanesulfonic acid (MSA) concentration, time of leaching reaction, temperature, liquid/solid ratio (L/S) and stirring speed on dissolution of valuable elements in MSA were studied. The optimized conditions for dissolution of various metals were: methanesulfonic acid concentration; 150g/L, dissolution time; 300 min, temperature; 363K, liquid to solid ratio; 4 ml/g and stirring speed; 400 rpm. The dissolution efficiency of Zn, Cu, Ni and Pb are 81.8%, 79.47%, 76.6%, and 70.7%, respectively under the optimal conditions. Different mathematical kinetic models for the dissolution process in MSA were studied since it is very important for economic metal dissolution. The experimental data were best fitted by pseudo-second-order homogeneous reaction model for zinc (Zn), copper (Cu) and nickel (Ni), whilst lead (Pb) was best fitted by the diffusion through the product or ash layer. The activation energies of the dissolution processes of different metals were evaluated. Overall, the MSA leaching system provides an efficient, clean and green method for dissolution of valuable metals. It can be a promising alternative to inorganic acids. GRAPHICAL ABSTRACT
{"title":"Efficient Leaching Process of Valuable Elements from Gibbsite Ore Materials in Talet Seleim, Southwestern, Sinai, Egypt Using Green and Ecofriendly Lixiviant Agent: Optimization, Kinetic and Thermodynamic Study","authors":"A. Salem","doi":"10.1080/22297928.2023.2222281","DOIUrl":"https://doi.org/10.1080/22297928.2023.2222281","url":null,"abstract":"Abstract Here, valuable elements in Talet Seleim, Southwestern Sinai, Egypt, were leached using methanesulfonic acid (MSA) as an environmentally friendly lixiviant agent. The effects of methanesulfonic acid (MSA) concentration, time of leaching reaction, temperature, liquid/solid ratio (L/S) and stirring speed on dissolution of valuable elements in MSA were studied. The optimized conditions for dissolution of various metals were: methanesulfonic acid concentration; 150g/L, dissolution time; 300 min, temperature; 363K, liquid to solid ratio; 4 ml/g and stirring speed; 400 rpm. The dissolution efficiency of Zn, Cu, Ni and Pb are 81.8%, 79.47%, 76.6%, and 70.7%, respectively under the optimal conditions. Different mathematical kinetic models for the dissolution process in MSA were studied since it is very important for economic metal dissolution. The experimental data were best fitted by pseudo-second-order homogeneous reaction model for zinc (Zn), copper (Cu) and nickel (Ni), whilst lead (Pb) was best fitted by the diffusion through the product or ash layer. The activation energies of the dissolution processes of different metals were evaluated. Overall, the MSA leaching system provides an efficient, clean and green method for dissolution of valuable metals. It can be a promising alternative to inorganic acids. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"41 1","pages":"141 - 158"},"PeriodicalIF":0.0,"publicationDate":"2023-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85153808","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-03-04DOI: 10.1080/22297928.2023.2217176
Swati Bharati, Vinod L. Gaikwad, Bothiraja Chellampillai
Abstract Famotidine (FAM), a histamine H2 receptor antagonist, is effective against peptic ulcers and Zollinger Ellison syndrome. In the current investigation, a HPLC approach was developed to detect the Famotidine (FAM) in pre-clinical samples (rat plasma). To get rid of any chromatographic solvent effects, methanolic extraction method was used to prepare biological samples. A C18 column was used for chromatographic separation, with a pH-adjusted to 8 as mobile phase of water, methanol, and acetonitrile (70: 20: 10, v/v/v) at a flow rate of 1 mL/min and UV detection at 264 nm. The retention times of FAM was found to be 5.7 min. The technique was linear in the range of 50 to 1400 ng/mL in plasma concentration with R2 of 0.9985. The newly proposed method’s respective limits for quantification and detection were found to be 151.45 ± 6.47 ng/mL and 49.97 ± 2.14 ng/mL. The average recovery rates were discovered to range from 98.06 to 103.56%. After numerous freeze-thaw cycles of the treated plasma samples, analyte was stable and showed no sign of significant deterioration. After a single oral dose of 10 mg/kg of FAM, the approach was effectively used to assess the pharmacokinetic characteristics in Wistar albino rats. Consequently, the straightforward technique would enable quick with affordable detection of the FAM from biological samples. GRAPHICAL ABSTRACT
{"title":"Investigation of a Quantitative Bioanalytical HPLC Method for the Assessment of Famotidine in Pre-clinical Samples: Application for Pharmacokinetic Studies","authors":"Swati Bharati, Vinod L. Gaikwad, Bothiraja Chellampillai","doi":"10.1080/22297928.2023.2217176","DOIUrl":"https://doi.org/10.1080/22297928.2023.2217176","url":null,"abstract":"Abstract Famotidine (FAM), a histamine H2 receptor antagonist, is effective against peptic ulcers and Zollinger Ellison syndrome. In the current investigation, a HPLC approach was developed to detect the Famotidine (FAM) in pre-clinical samples (rat plasma). To get rid of any chromatographic solvent effects, methanolic extraction method was used to prepare biological samples. A C18 column was used for chromatographic separation, with a pH-adjusted to 8 as mobile phase of water, methanol, and acetonitrile (70: 20: 10, v/v/v) at a flow rate of 1 mL/min and UV detection at 264 nm. The retention times of FAM was found to be 5.7 min. The technique was linear in the range of 50 to 1400 ng/mL in plasma concentration with R2 of 0.9985. The newly proposed method’s respective limits for quantification and detection were found to be 151.45 ± 6.47 ng/mL and 49.97 ± 2.14 ng/mL. The average recovery rates were discovered to range from 98.06 to 103.56%. After numerous freeze-thaw cycles of the treated plasma samples, analyte was stable and showed no sign of significant deterioration. After a single oral dose of 10 mg/kg of FAM, the approach was effectively used to assess the pharmacokinetic characteristics in Wistar albino rats. Consequently, the straightforward technique would enable quick with affordable detection of the FAM from biological samples. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"15 1","pages":"202 - 212"},"PeriodicalIF":0.0,"publicationDate":"2023-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77060679","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-03-04DOI: 10.1080/22297928.2023.2222311
P. Khurana, S. Lingayat, S. Thatai
Abstract This study deals with the different shape and sizes of silica nanoparticles (SiO2 NPs) ranging from a typical sphere to Y-shape to core-shell. The particles have been categorized as three i.e., mesoporous, macroporous and core-shell. Stöber process has played a great role in the fabrication of SiO2 NPs and by varying parameters like surfactant, solvent, pH, templating techniques, water to surfactant ratio, surfactant to co-surfactant ratio etc., the morphology was observed to change. The modified SiO2 NPs obtained were spherical and changed to rod shape and then to Y-shape with change in concentration of alcohol. The effect of above reaction parameters has been investigated on size and shape of NPs which is further discussed in review. SiO2 NPs in form of composites are widely used in the field of bio-sensing, adsorbents, water treatment, drug delivery etc. This review article aims to present different shapes of SiO2 NPs and discuss its application as an adsorbent for water remediation techniques. GRAPHICAL ABSTRACT
{"title":"Synthesis of Silica Spherical to Y-Shape Nanoparticles: A Review with Surface Modifications and Its Characterization","authors":"P. Khurana, S. Lingayat, S. Thatai","doi":"10.1080/22297928.2023.2222311","DOIUrl":"https://doi.org/10.1080/22297928.2023.2222311","url":null,"abstract":"Abstract This study deals with the different shape and sizes of silica nanoparticles (SiO2 NPs) ranging from a typical sphere to Y-shape to core-shell. The particles have been categorized as three i.e., mesoporous, macroporous and core-shell. Stöber process has played a great role in the fabrication of SiO2 NPs and by varying parameters like surfactant, solvent, pH, templating techniques, water to surfactant ratio, surfactant to co-surfactant ratio etc., the morphology was observed to change. The modified SiO2 NPs obtained were spherical and changed to rod shape and then to Y-shape with change in concentration of alcohol. The effect of above reaction parameters has been investigated on size and shape of NPs which is further discussed in review. SiO2 NPs in form of composites are widely used in the field of bio-sensing, adsorbents, water treatment, drug delivery etc. This review article aims to present different shapes of SiO2 NPs and discuss its application as an adsorbent for water remediation techniques. GRAPHICAL ABSTRACT","PeriodicalId":7793,"journal":{"name":"Analytical Chemistry Letters","volume":"42 1","pages":"106 - 126"},"PeriodicalIF":0.0,"publicationDate":"2023-03-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87053458","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}
京公网安备 11010802042870号
京ICP备2023020795号-1
扫码关注我们
求助内容：
应助结果提醒方式：