SEPARATION SCIENCE PLUS最新文献_第8页

Designing a bacterial cellulose‐based hydrogel incorporated with manganese sulfide and graphene oxide for green extraction of acrylamide in bread samples 设计一种含有硫化锰和氧化石墨烯的细菌纤维素基水凝胶，用于面包样品中丙烯酰胺的绿色提取

SEPARATION SCIENCE PLUS Pub Date : 2023-10-20 DOI: 10.1002/sscp.202300169

Hassan Sereshti, Fatemeh Rezvani, Sara Soltani, Faezeh Karami, Hamid Rashidi Nodeh

{"title":"Designing a bacterial cellulose‐based hydrogel incorporated with manganese sulfide and graphene oxide for green extraction of acrylamide in bread samples","authors":"Hassan Sereshti, Fatemeh Rezvani, Sara Soltani, Faezeh Karami, Hamid Rashidi Nodeh","doi":"10.1002/sscp.202300169","DOIUrl":"https://doi.org/10.1002/sscp.202300169","url":null,"abstract":"Abstract A novel nanocomposite based on bacterial cellulose (BC) modified by manganese sulfide (MnS) decorated graphene oxide (GO) was prepared. The hydrogel was characterized by Fourier transform infrared, scanning electron microscopy, energy‐dispersive X‐ray spectroscopy, and adsorption/desorption techniques. The sorbent was employed for determining acrylamide in bread samples using micro‐solid‐phase extraction coupled with high‐performance liquid chromatography. The extraction efficiency of prepared sorbent was 1.4‐fold higher than that of BC. The important extraction factors including elution conditions (acetonitrile 300 μL, 5 min), sorbent composition and mass (50 mg), adsorption time (7 min), sample solution pH (8), and salt effect (3% w/v) were considered for optimization of the method. The analytical merit was validated by assessing the preconcentration factor (178–225), limit of detection (1.56 μg/kg), limit of quantification (5.15 μg/kg), linearity (5.15–500 μg/kg), and determination coefficient (0.9845). The adsorption isotherms and kinetic studies demonstrated that the adsorption process followed the Langmuir model and pseudo‐second‐order kinetics. The relative recoveries and relative standard deviations were 84%–106% and 2.4%–9.2%, respectively. This paper is the first report on the fabrication and use of BC doped with MnS‐GO composite for extraction of acrylamide in typical commercial bread samples.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135567500","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}

引用次数: 0

Detection of synthetic lipid‐lowering adulterants in herbal products using high‐performance thin‐layer chromatography 高效薄层色谱法检测中药产品中合成降脂掺假物

SEPARATION SCIENCE PLUS Pub Date : 2023-10-20 DOI: 10.1002/sscp.202300165

Hardi Joshi, Payal Bahliwala, Jigna Vadalia, Udaykumar Vegad

{"title":"Detection of synthetic lipid‐lowering adulterants in herbal products using high‐performance thin‐layer chromatography","authors":"Hardi Joshi, Payal Bahliwala, Jigna Vadalia, Udaykumar Vegad","doi":"10.1002/sscp.202300165","DOIUrl":"https://doi.org/10.1002/sscp.202300165","url":null,"abstract":"Abstract Adulterating herbal medicine with undeclared synthetic drugs is a worldwide problem that seriously threatens human health. To detect such illicit and not labeled synthetic hypolipidemic substances in herbal medicines, an analytical method to simultaneously identify and quantify atorvastatin (ATV) calcium, simvastatin (SIM), gemfibrozil (GEM), fenofibrate (FEN) belonging to two different classes of drugs (statins and fibrates) was developed based on high‐performance thin‐layer chromatography. The method consisted of Silica Gel G60 F 254 precoated aluminum plate as stationary phase and toluene: ethyl acetate: formic acid (7:3:0.3, v/v/v) as optimized mobile phase. The densitometric evaluation wavelength was optimized at 254 nm. The Rf values of ATV, SIM, GEM, and FEN were 0.157, 0.268, 0.691, and 0.852, respectively. The linearity range is between 100–1500 ng/band for ATV and FEN and 200–3000 ng/band for SIM and GEM, respectively. The accuracy was found to be in the range of 97%–105%. The relative standard deviation of precision and robustness was found to be < 5%. However, the five screened market samples did not show the presence of adulteration of the above drugs. This method for the simultaneous determination of four drugs may be successfully employed to screen synthetic hypolipidemics as adulterants in herbal products and dietary supplements.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135616659","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}

引用次数: 0

Simultaneous estimation of propyphenazone, flurbiprofen, and their mutual prodrug by high‐performance liquid chromatography method 高效液相色谱法同时测定丙苯那酮、氟比洛芬及其相互前药的含量

SEPARATION SCIENCE PLUS Pub Date : 2023-10-19 DOI: 10.1002/sscp.202300104

Zanza Patel, Falguni Tandel, Rati Kailash Prasad Tripathi

{"title":"Simultaneous estimation of propyphenazone, flurbiprofen, and their mutual prodrug by high‐performance liquid chromatography method","authors":"Zanza Patel, Falguni Tandel, Rati Kailash Prasad Tripathi","doi":"10.1002/sscp.202300104","DOIUrl":"https://doi.org/10.1002/sscp.202300104","url":null,"abstract":"Abstract The current work comprises of development of a simple, rapid, and precise reverse phase‐high‐performance liquid chromatography method for simultaneous estimation of propyphenazone, flurbiprofen, and their mutual prodrug. Column C18 (Shimadzu Shim‐pack Gist, 250 × 4.6 mm, 5 μm) was employed as a stationary phase, and the ratio of acetonitrile:methanol:water (40:40:20 %v/v) was used as the mobile phase. The flow rate was held at 1 mL/min and detection was carried out at 245 nm using an ultraviolet detector. The retention time of propyphenazone, flurbiprofen, and their mutual prodrug was found to be 4.0, 2.5, and 10.0 min, respectively. The proposed method was validated according to the International Council on Harmonization Q2(R1) guideline in terms of accuracy, precision, linearity, limit of detection, limit of quantitation, and solution stability. Calibration plots were linear over the concentration ranges of 2–10 μg/mL (R 2 = 0.9998, R 2 = 0.9992 and R 2 = 0.9994 for propyphenazone, flurbiprofen, and their mutual prodrug, respectively). Results of mean percentage recoveries were in the range of 99.6%–100.1% for flurbiprofen, 99.3%–100.2% for propyphenazone, and 99.9%–100.7% for prodrug, respectively. The developed method can be used for the assay of mutual prodrug and drug release study of the developed mutual prodrug also routine quality control evaluation of mutual prodrug in bulk form.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135729330","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}

引用次数: 0

Solid‐phase extraction of losartan and chlordiazepoxide from biological samples using sponge‐activated carbon 海绵活性炭固相萃取生物样品中的氯沙坦和氯二氮环氧化物

SEPARATION SCIENCE PLUS Pub Date : 2023-10-10 DOI: 10.1002/sscp.202300096

Saeid Khodadoust, Ferdous Pirayesh, Fatemeh Zeraatpisheh

{"title":"Solid‐phase extraction of losartan and chlordiazepoxide from biological samples using sponge‐activated carbon","authors":"Saeid Khodadoust, Ferdous Pirayesh, Fatemeh Zeraatpisheh","doi":"10.1002/sscp.202300096","DOIUrl":"https://doi.org/10.1002/sscp.202300096","url":null,"abstract":"Abstract In this research, sponge‐activated carbon was applied as an effective adsorbent for simultaneous dispersive solid ultrasound‐assisted microextraction followed by high‐performance liquid chromatography for the preconcentration and determination of losartan (LOS) and chlordiazepoxide (CDP) drugs from urine and plasma samples. The synthesized adsorbent was characterized using scanning electron microscopy and Brunauer–Emmett–Teller techniques. To investigate the effects of different parameters, such as adsorbent dosage, pH, adsorption time, and volume of extraction solvent on the extraction process of LOS and CDP, a central composite design (CCD)‐based response surface methodology was applied. Using a CCD, the optimized factors achieved an adsorption time of 13 min, an adsorbent dosage of 14 mg, an extraction solvent (methanol) of 1.3 mL, and pH = 4.7 under the desirability function. Under the optimized conditions, the presented method showed a wide linear range of 0.005–10.0 μg/mL with a limit of detections of 0.0011 and 0.0018 μg/mL for LOS and CDP, respectively. Moreover, the applied method had relative standard deviations of 4.7% and 5.3% for LOS and CDP, respectively.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"136359835","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}

引用次数: 0

A novel method for the extraction and characterization of metabolites from Basidiomycota: Pleurotus ostreatus (Jacq.) P. Kumm., 1871 as a case study 担子菌(Pleurotus ostreatus)代谢物的提取与鉴定新方法p . Kumm。1871年作为案例研究

SEPARATION SCIENCE PLUS Pub Date : 2023-10-10 DOI: 10.1002/sscp.202300116

Mirko Benvenuti, Simone Di Piazza, Annalisa Salis, Grazia Cecchi, Mirca Zotti, Sonia Scarfì, Gianluca Damonte

{"title":"A novel method for the extraction and characterization of metabolites from Basidiomycota: Pleurotus ostreatus (Jacq.) P. Kumm., 1871 as a case study","authors":"Mirko Benvenuti, Simone Di Piazza, Annalisa Salis, Grazia Cecchi, Mirca Zotti, Sonia Scarfì, Gianluca Damonte","doi":"10.1002/sscp.202300116","DOIUrl":"https://doi.org/10.1002/sscp.202300116","url":null,"abstract":"Abstract In recent years, the interest in the exploitation of fungal metabolites has grown considerably, given their application in numerous sectors involving human health. However, their identification and characterization by conventional analytical approaches is generally limited to single families of molecules per method of analysis. This constitutes a limiting factor of primary importance in the study of both the metabolic pattern of a single fungal sample and the discovery of its possible applications. In this work, a reverse‐phase high‐performance liquid chromatography coupled with mass spectrometry method for the profile determination of primary and secondary metabolites produced by the oyster‐mushroom Pleurotus ostreatus (Jacq.) P. Kumm., 1871, has been developed. By using a concomitant extraction in three different polarity‐decreasing solvents, namely methanol, ethanol, and acetonitrile, this method allowed the simultaneous analysis of all extracted metabolites belonging to the widest possible range of chemical families, giving an advantage for both qualitative and quantitative determination of known and unknown compounds. The method appears to be valuable and robust for the study of complex matrices like raw fungi extract such as those of Pleurotus ostreatu s cultivated on different substrates and/or exposed to multiple stressors.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"136353389","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}

引用次数: 0

Simultaneous detection and analysis of 11 nootropic compounds in 54 samples via liquid chromatography‐electrospray ionization‐tandem mass spectrometry and quadrupole time‐of‐flight mass spectrometry 采用液相色谱-电喷雾电离-串联质谱法和四极杆飞行时间质谱法对54个样品中的11种促智化合物进行了同时检测和分析

SEPARATION SCIENCE PLUS Pub Date : 2023-10-09 DOI: 10.1002/sscp.202300127

Nam Sook Kim, Hwan Seong Choi, Hyunil Shin, Ji Hyun Lee, Hyungil Kim, Sooyeul Cho

{"title":"Simultaneous detection and analysis of 11 nootropic compounds in 54 samples via liquid chromatography‐electrospray ionization‐tandem mass spectrometry and quadrupole time‐of‐flight mass spectrometry","authors":"Nam Sook Kim, Hwan Seong Choi, Hyunil Shin, Ji Hyun Lee, Hyungil Kim, Sooyeul Cho","doi":"10.1002/sscp.202300127","DOIUrl":"https://doi.org/10.1002/sscp.202300127","url":null,"abstract":"Abstract Dietary supplements used for improving brain function and strengthening attention are increasingly popular. However, illegal dietary supplements containing unapproved drugs continue to be seized. Therefore, it is necessary to rapidly screen and identify adulterated compounds in dietary supplements for public safety. To develop the simultaneous analytical method, we selected 11 nootropic compounds and optimized the simultaneous liquid chromatography‐electrospray ionization‐tandem mass spectrometry and optimal conditions for liquid chromatography‐quadrupole time‐of‐flight mass spectrometry were proposed to determine the fragmentation patterns of each compound. The specificity, linearity, limit of detection, limit of quantification, method detection limit, method quantitation limit, precision, accuracy, matrix effect, and stability of this method were evaluated according to international validation guidelines. The validated methods were applied to 54 samples containing dietary supplements and seized samples. On screening 11 nootropic compounds were detected in four solid samples (tablet and powder). By comparing the product ion ratios with the standards and quantification, vinpocetine (6.52–34.2 mg/g) was found in three samples, and omberacetam (995.6 mg/g) in one sample. To re‐confirm the detected compounds, the fragmentation patterns were compared with those of the standards using liquid chromatography‐quadrupole time‐of‐flight mass spectrometry. The developed simultaneous analysis method can help maintain public health and safety.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-10-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135092807","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}

引用次数: 0

Synthesis and application of dual‐layer metal‐organic framework as a fiber coating based on copper‐based metal‐organic framework @ zeolitic imidazolate framework‐8 for solid‐phase microextraction of some selected parabens and their quantification using high performance liquid chromatography 基于铜基金属-有机骨架@沸石咪唑酯骨架- 8的双层金属-有机骨架纤维涂层的合成和应用，用于固相微萃取某些对羟基苯甲酸酯及其高效液相色谱定量分析

SEPARATION SCIENCE PLUS Pub Date : 2023-10-05 DOI: 10.1002/sscp.202300141

Abeer Fadhil Mohammed, Milad Ghani, Jahan Bakhsh Raoof

{"title":"Synthesis and application of dual‐layer metal‐organic framework as a fiber coating based on copper‐based metal‐organic framework @ zeolitic imidazolate framework‐8 for solid‐phase microextraction of some selected parabens and their quantification using high performance liquid chromatography","authors":"Abeer Fadhil Mohammed, Milad Ghani, Jahan Bakhsh Raoof","doi":"10.1002/sscp.202300141","DOIUrl":"https://doi.org/10.1002/sscp.202300141","url":null,"abstract":"Abstract Herein, the zeolitic imidazolate framework‐8 template was accommodated onto the surface of a pencil graphite substrate through the electrodeposition system. Then, Zn in the zeolitic imidazolate framework‐8 was replaced with Cu atoms via the galvanic replacement procedure. The modified template was used for the synthesis of another metal‐organic framework (copper‐benzene di carboxylic acid) by a solvothermal method. The prepared fiber was characterized by field emission‐scanning electron microscopy, Fourier transform infrared spectroscopy, and X‐ray diffraction technique. Then, it was employed for direct immersion solid‐phase microextraction of methyl, ethyl, and butyl parabens. Various factors, such as the pH of the sample solution, stirring rate, desorption volume, the concentration of salt, extraction time, and desorption time, were selected and optimized. Under the optimized condition (extraction time = 30 min, desorption time = 2 min, desorption volume = 200 μL, salt concentration = 0% w/v, sample solution pH = 3.0, and stirring rate = 700 rpm), the linearity of the method was in the range of 1–200 μg/L ( r 2 > 0.9926). The limits of detection and quantification fall between 0.28–0.65 μg/L and 0.91–1.98 μg/L, respectively. The analysis of selected parabens in toothpaste and hand and face lotion, were also done using the suggested methodology.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","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":"134973675","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}

引用次数: 0

A systematic review on bisphenols – Sources, health impacts, and analytical determination of bisphenol A in aqueous samples 双酚的来源、对健康的影响和水样中双酚A的分析测定的系统综述

SEPARATION SCIENCE PLUS Pub Date : 2023-09-29 DOI: 10.1002/sscp.202300072

Veena Vinod, Amritha P S, Harathi P B

{"title":"A systematic review on bisphenols – Sources, health impacts, and analytical determination of bisphenol A in aqueous samples","authors":"Veena Vinod, Amritha P S, Harathi P B","doi":"10.1002/sscp.202300072","DOIUrl":"https://doi.org/10.1002/sscp.202300072","url":null,"abstract":"Abstract Bisphenol A and its structural analogs are used by industrial processes for the manufacture of plastics, and medical and electronic devices. When these products are disposed of, they tend to leach out causing pollution and impacting human health. Thus, many studies are focused on detecting the presence of Bisphenols in environmental matrices, especially in water and food, as it is a major route of human exposure. Advancements have been made in the preparation and detection of samples using different analytical techniques. The most widely used techniques for bisphenol detection are liquid chromatography and gas chromatography coupled with mass spectroscopy. The progress made for ultra‐trace detection of Bisphenols via the development of efficient sample extraction techniques and the benefits of each technique are highlighted. The recent advances in detection techniques using colorimetric and Raman spectroscopy are reviewed with an emphasis on the use of portable onsite techniques compared to conventional labor‐intensive and time‐consuming techniques. An overview of all the approaches to determining Bisphenols in environmental and food samples is discussed in detail to provide insight into the progress made in this field.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-09-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135244041","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}

引用次数: 0

Rapid identification of chemical constituents of Chaihu‐jia‐Longgu‐Muli decoction based on ultra‐performance liquid chromatography‐quadrupole time‐of‐flight mass spectrometry coupled with the UNIFI platform 基于超高效液相色谱-四极杆飞行时间质谱联用UNIFI平台快速鉴定柴胡-佳-龙骨-木里汤的化学成分

SEPARATION SCIENCE PLUS Pub Date : 2023-09-22 DOI: 10.1002/sscp.202300103

Tong Wu, Yin Liu, Hanshuo Dong, Chunling Ai, Li Sun

{"title":"Rapid identification of chemical constituents of Chaihu‐jia‐Longgu‐Muli decoction based on ultra‐performance liquid chromatography‐quadrupole time‐of‐flight mass spectrometry coupled with the UNIFI platform","authors":"Tong Wu, Yin Liu, Hanshuo Dong, Chunling Ai, Li Sun","doi":"10.1002/sscp.202300103","DOIUrl":"https://doi.org/10.1002/sscp.202300103","url":null,"abstract":"Abstract Chaihu‐jia Longgu‐Muli decoction (CLMD) is a traditional Chinese medicine formula, and it has been used for more than a thousand years to treat mental and nervous system diseases. However, the active constitutions of the CLMD are unclear. Accordingly, an integrated analysis based on the ultra‐performance liquid chromatography‐quadrupole time‐of‐flight mass spectrometry method combined with the UNIFI platform was used to clarify the chemical composition of the CLMD. As a result, 102 compounds including 38 saponins, 32 flavonoids, 12 polyphenols, nine anthraquinones, and 11 others were identified or tentatively presumed. Among them, 19 compounds were confirmed unambiguously with standards. Moreover, the characteristic fragmentations and fragmentation patterns of different compounds in CLMD were summarized, and each compound was classified as an individual herb. It was demonstrated that this method is rapid and accurate and could provide a strategy for the qualitative analysis of the chemical constituents of CLMD, and these results will provide experimental evidence for the subsequent studies on the pharmacodynamic material basis and quality control of CLMD.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-09-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"136061358","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}

引用次数: 0

Separation and quantitation of valacyclovir enantiomers using stability‐indicating chiral liquid chromatography method with a chiral stationary phase of amylose tris‐(3,5‐dimethylphenylcarbamate) 以直链淀粉三(3,5 -二甲基苯基氨基甲酸酯)为手性固定相，稳定性指示手性液相色谱法分离和定量伐昔洛韦对映体

SEPARATION SCIENCE PLUS Pub Date : 2023-09-21 DOI: 10.1002/sscp.202300145

Niroja Vadagam, Sharath Babu Haridasyam, Muvvala Venkatanarayana, Narasimha S. Lakka, Sanjeeva R. Chinnakadoori

{"title":"Separation and quantitation of valacyclovir enantiomers using stability‐indicating chiral liquid chromatography method with a chiral stationary phase of amylose tris‐(3,5‐dimethylphenylcarbamate)","authors":"Niroja Vadagam, Sharath Babu Haridasyam, Muvvala Venkatanarayana, Narasimha S. Lakka, Sanjeeva R. Chinnakadoori","doi":"10.1002/sscp.202300145","DOIUrl":"https://doi.org/10.1002/sscp.202300145","url":null,"abstract":"Abstract The present research developed and validated a new stability‐indicating technique for the stereo‐selectively enantiomers of the antiviral nucleoside analog Valacyclovir hydrochloride (VAL). The chiral separation was performed using normal‐phase high‐performance liquid chromatography (HPLC) with a chiral stationary phase consisting of amylose tris(3‐chloro‐5‐methylphenylcarbamate) and a mobile phase of “ n ‐hexane, methanol, ethanol, and diethylamine”, flow rate of 0.60 mL/min, column temperature of 30°C, injection volume of 10‐μL, detection wavelength of 254‐nm, and run time of 25‐min. The enantiomers (S‐enantiomer, L‐isomer, R‐enantiomer, and D‐isomer) of Valacyclovir were separated with a resolution of 4.8 and no interference. The validation parameters verified for the proposed method, linearity in a range of 0.1002–24.3486 μg/mL (0.02–4.86%) with a regression coefficient of 0.999, and the accuracy was determined with excellent recoveries ranging from 94.38%–109.97%. The concentrations established for the detection limit and quantitation limit were 0.01% and 0.02%, respectively. The forced degradation experiments were used to assess the stability‐indicating qualities. D‐Valacyclovir impurity was successfully evaluated in release and stability samples of VAL in drug substance and tablet dosage forms using the proposed normal phase chiral HPLC approach.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-09-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"136155039","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}

引用次数: 2