Osama A. Mahmoud, Ahmed A. Omran, Hosni A. Gomaa, Mahmoud A. Mohamed
Abstract Doxycycline hyclate (DOXH) is very important to treat acne and prevent infections caused by bacteria, so quantifying doxycycline hyclate and its related substances is crucial. In this work, All analytes of doxycycline and its related substances, including methacycline, 4‐epi doxycycline, 6‐epi doxycycline, and 2‐acetyl‐2‐carbamoyl doxycycline, were successfully separated at low concentrations in a single run utilizing the suggested isocratic high‐performance liquid chromatography method with a mobile phase comprising water:acetonitrile:perchloric acid (75:25:0.2, v/v), Phenomenex Luna C18 column (50 × 4.6 mm, 3 μm i.d.) maintained at 30°C with a flow rate of 0.7 mL/min, injection volume of 25 μL, and photodiode array detector at 269 nm. DOXH and its related substances were linear in the range of 0.25–50, 0.1–30, 0.2–35, 0.5–50, and 0.6–20 μg/mL, respectively, with correlation coefficients greater than 0.999 and good accuracy results between 98% and 102%. The method has been successfully used to determine the drug's comparative study in both generic and reference products, demonstrating the similarity between the two products. According to the International Council for Harmonization requirements, the proposed approach was validated. Additionally, the technique has effectively studied in vitro dissolution, Six Sigma, and content uniformity.
{"title":"Stability indicating high‐performance liquid chromatography method for determining doxycycline hyclate and related substances in their various dosage forms: Utilizing Six Sigma tools, uniformity testing, and in‐vitro dissolution approaches","authors":"Osama A. Mahmoud, Ahmed A. Omran, Hosni A. Gomaa, Mahmoud A. Mohamed","doi":"10.1002/sscp.202300173","DOIUrl":"https://doi.org/10.1002/sscp.202300173","url":null,"abstract":"Abstract Doxycycline hyclate (DOXH) is very important to treat acne and prevent infections caused by bacteria, so quantifying doxycycline hyclate and its related substances is crucial. In this work, All analytes of doxycycline and its related substances, including methacycline, 4‐epi doxycycline, 6‐epi doxycycline, and 2‐acetyl‐2‐carbamoyl doxycycline, were successfully separated at low concentrations in a single run utilizing the suggested isocratic high‐performance liquid chromatography method with a mobile phase comprising water:acetonitrile:perchloric acid (75:25:0.2, v/v), Phenomenex Luna C18 column (50 × 4.6 mm, 3 μm i.d.) maintained at 30°C with a flow rate of 0.7 mL/min, injection volume of 25 μL, and photodiode array detector at 269 nm. DOXH and its related substances were linear in the range of 0.25–50, 0.1–30, 0.2–35, 0.5–50, and 0.6–20 μg/mL, respectively, with correlation coefficients greater than 0.999 and good accuracy results between 98% and 102%. The method has been successfully used to determine the drug's comparative study in both generic and reference products, demonstrating the similarity between the two products. According to the International Council for Harmonization requirements, the proposed approach was validated. Additionally, the technique has effectively studied in vitro dissolution, Six Sigma, and content uniformity.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-11-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"134991753","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}
Abstract High‐performance thin‐layer chromatography (HPTLC), a top‐notch technique in the field of analysis, is quite irreplaceable when it comes to identifying and standardizing medicinal plants . Marsdenia tenacissima and Leptadenia reticulata have claimed traditional uses like anti‐cancer, anti‐inflammatory, anti‐depressant, hepatoprotection, etc., with few similar phytoconstituents. In this study, a precise and validated HPTLC densitometric method was developed for the identification of α‐amyrin, β‐sitosterol, and betulin in the above‐mentioned plants by static maceration with ethanol and aqueous‐ethanol extracts. The developed method was evaluated by linearity, range, accuracy, precision, limit of detection, limit of quantification, robustness, and specificity. The markers were subjected to ascending development with toluene: ethyl acetate: glacial acetic acid at a ratio of 8:1.5:0.5 v/v/v, air‐dried, and derivatized with anisaldehyde‐sulfuric acid. The retardation factor values of the markers were found to be 0.63 (α‐amyrin), 0.52 (β‐sitosterol), and 0.64 (betulin) for L. reticulata , and 0.55 (α‐amyrin), 0.45 (β‐sitosterol), and 0.57 (betulin) for M. tenacissima . The chromatographic results suggest that the developed method suits all three markers and can be simultaneously identified in both plants.
{"title":"Development and validation of high‐performance thin‐layer chromatography method for simultaneous estimation of α‐Amyrin, Betulin, and β‐Sitosterol in <i>Leptadenia reticulata</i> and <i>Marsdenia tenacissima</i>","authors":"Sahaya Mercy Jaquline Robert, Vidhu Aeri","doi":"10.1002/sscp.202300092","DOIUrl":"https://doi.org/10.1002/sscp.202300092","url":null,"abstract":"Abstract High‐performance thin‐layer chromatography (HPTLC), a top‐notch technique in the field of analysis, is quite irreplaceable when it comes to identifying and standardizing medicinal plants . Marsdenia tenacissima and Leptadenia reticulata have claimed traditional uses like anti‐cancer, anti‐inflammatory, anti‐depressant, hepatoprotection, etc., with few similar phytoconstituents. In this study, a precise and validated HPTLC densitometric method was developed for the identification of α‐amyrin, β‐sitosterol, and betulin in the above‐mentioned plants by static maceration with ethanol and aqueous‐ethanol extracts. The developed method was evaluated by linearity, range, accuracy, precision, limit of detection, limit of quantification, robustness, and specificity. The markers were subjected to ascending development with toluene: ethyl acetate: glacial acetic acid at a ratio of 8:1.5:0.5 v/v/v, air‐dried, and derivatized with anisaldehyde‐sulfuric acid. The retardation factor values of the markers were found to be 0.63 (α‐amyrin), 0.52 (β‐sitosterol), and 0.64 (betulin) for L. reticulata , and 0.55 (α‐amyrin), 0.45 (β‐sitosterol), and 0.57 (betulin) for M. tenacissima . The chromatographic results suggest that the developed method suits all three markers and can be simultaneously identified in both plants.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-11-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"136351447","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}
Mohan Pasham, Sharath Babu Haridasyam, Niroja Vadagam, N. V. V. D. Praveen Boppy, Sanjeeva R. Chinnakadoori, Narasimha S. Lakka
Abstract Propranolol hydrochloride (PPH) is a medication of beta‐adrenergic receptors. It is used to treat pediatric hemangiomas that are growing and need systemic therapy. A reversed‐phase high‐performance liquid chromatography (HPLC) was made to separate and estimate the amounts of ten known organic impurities of propranolol in bulk drugs, tablets, and capsule dosage forms. The chromatographic separation was achieved on a C 18 column (100 × 4.6 mm, 2.7 μm) using a binary gradient mixture of pH 2.3 phosphate buffer and organic modifiers of acetonitrile, methanol, and isopropyl alcohol as the mobile phase. The stability‐indicating character of the proposed method was proven using stress testing study. The test method was validated for specificity, limit of detection, limit of quantitation, linearity, precision, accuracy, and robustness. For the propranolol and its ten organic impurities, the limit of quantitation, linearity, and recoveries were found in a range of 0.0123–0.4266 μg/mL ( R 2 > 0.9982) and 89.2–98.9%, respectively. The proposed liquid chromatography method is found to be highly suitable for impurity profiling of propranolol in bulk drugs and pharmaceutical formulations (tablets and capsules).
{"title":"Separation and quantification of organic‐related impurities of beta‐adrenergic receptor blocking agent propranolol in pharmaceutical solid dosage forms: Impurity profiling using stability‐indicating HPLC method","authors":"Mohan Pasham, Sharath Babu Haridasyam, Niroja Vadagam, N. V. V. D. Praveen Boppy, Sanjeeva R. Chinnakadoori, Narasimha S. Lakka","doi":"10.1002/sscp.202300159","DOIUrl":"https://doi.org/10.1002/sscp.202300159","url":null,"abstract":"Abstract Propranolol hydrochloride (PPH) is a medication of beta‐adrenergic receptors. It is used to treat pediatric hemangiomas that are growing and need systemic therapy. A reversed‐phase high‐performance liquid chromatography (HPLC) was made to separate and estimate the amounts of ten known organic impurities of propranolol in bulk drugs, tablets, and capsule dosage forms. The chromatographic separation was achieved on a C 18 column (100 × 4.6 mm, 2.7 μm) using a binary gradient mixture of pH 2.3 phosphate buffer and organic modifiers of acetonitrile, methanol, and isopropyl alcohol as the mobile phase. The stability‐indicating character of the proposed method was proven using stress testing study. The test method was validated for specificity, limit of detection, limit of quantitation, linearity, precision, accuracy, and robustness. For the propranolol and its ten organic impurities, the limit of quantitation, linearity, and recoveries were found in a range of 0.0123–0.4266 μg/mL ( R 2 > 0.9982) and 89.2–98.9%, respectively. The proposed liquid chromatography method is found to be highly suitable for impurity profiling of propranolol in bulk drugs and pharmaceutical formulations (tablets and capsules).","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-11-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"136281867","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}
Abstract This study aimed to investigate the anti‐aging mechanism of raw and various processed Schisandrae chinensis fructus (SF) products by examining differences in serum metabolites in D‐galactose (D‐gal)‐induced aging rats. The study provides a metabolomic basis for SF as a tonic. The ultra‐high‐performance liquid chromatography‐Q‐time of flight‐tandem mass spectrometry technique was employed for serum metabolomic analysis of the anti‐aging effects of differently processed SF products. Multivariate statistical analysis, MetaboAnalyst, and Human Metabolome Database were utilized for pattern recognition and identification of characteristic metabolites. Enzyme‐linked immunosorbent assay results revealed significant differences between the aging model group and the blank group ( p < 0.01). Treatment with various processed SF products significantly improved related indicators in aging rats ( p < 0.05, p < 0.01). Arginine and seven other metabolites exhibited direct effects on aging. Wine‐processed Schisandrae (WS) treatment adjusted these biomarkers in aging rats to normal levels. WS significantly delayed D‐gal‐induced aging in rats by modulating endogenous biomarkers in relevant metabolic pathways, providing a scientific basis for its enhanced suitability as a tonic from a metabolomic perspective.
{"title":"Serum metabolomics study of anti‐aging mechanisms of different processed <i>Schisandra chinensis fructus</i> products","authors":"Jinyang Dai, Bo Pang, Hui Gao","doi":"10.1002/sscp.202300133","DOIUrl":"https://doi.org/10.1002/sscp.202300133","url":null,"abstract":"Abstract This study aimed to investigate the anti‐aging mechanism of raw and various processed Schisandrae chinensis fructus (SF) products by examining differences in serum metabolites in D‐galactose (D‐gal)‐induced aging rats. The study provides a metabolomic basis for SF as a tonic. The ultra‐high‐performance liquid chromatography‐Q‐time of flight‐tandem mass spectrometry technique was employed for serum metabolomic analysis of the anti‐aging effects of differently processed SF products. Multivariate statistical analysis, MetaboAnalyst, and Human Metabolome Database were utilized for pattern recognition and identification of characteristic metabolites. Enzyme‐linked immunosorbent assay results revealed significant differences between the aging model group and the blank group ( p < 0.01). Treatment with various processed SF products significantly improved related indicators in aging rats ( p < 0.05, p < 0.01). Arginine and seven other metabolites exhibited direct effects on aging. Wine‐processed Schisandrae (WS) treatment adjusted these biomarkers in aging rats to normal levels. WS significantly delayed D‐gal‐induced aging in rats by modulating endogenous biomarkers in relevant metabolic pathways, providing a scientific basis for its enhanced suitability as a tonic from a metabolomic perspective.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-11-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135291290","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}
Ashim Kumar Sen, Neel Bhimani, Dhanya B. Sen, Rajesh A. Maheshwari, Dipti Gohil, Shaileshkumar K. Koradia
Abstract A highly effective high‐performance thin‐layer chromatographic methodology has been developed and validated for the concurrent measurement of teneligliptin hydrobromide hydrate and pioglitazone hydrochloride in tablet offering excellent sensitivity, precision, accuracy, and robustness. The methodology involved using aluminum plates layered with silica gel 60F 254 were used, and the solvent system consisted of a mixture of chloroform, methanol, and ammonia (8:1:0.5 v/v/v). The analysis involved scanning of the plate at a wavelength of 229 nm and analyzing the resulting densitograms. The linear correlation was established over a range of concentrations 250–3000 ng/band for teneligliptin hydrobromide hydrate and 187.5–2250 ng/band for pioglitazone hydrochloride. The method displayed detection limits of 21.29 ng/band for teneligliptin hydrobromide hydrate and 25.97 ng/band for pioglitazone hydrochloride. The quantification limits were 64.52 ng/band for teneligliptin hydrobromide hydrate and 78.71 ng/band for pioglitazone hydrochloride. The results of precision parameters showed that the % relative standard deviation of peak area was consistently below 2%, indicating high precision. The accuracy of the method was demonstrated to be between 96% and 103%. Proposed method was found to be superior and capable of overcoming the shortcomings of previously reported methods for the assessment of both the drugs.
{"title":"Densitometric simultaneous assessment of teneligliptin hydrobromide and pioglitazone hydrochloride in combined tablet","authors":"Ashim Kumar Sen, Neel Bhimani, Dhanya B. Sen, Rajesh A. Maheshwari, Dipti Gohil, Shaileshkumar K. Koradia","doi":"10.1002/sscp.202300139","DOIUrl":"https://doi.org/10.1002/sscp.202300139","url":null,"abstract":"Abstract A highly effective high‐performance thin‐layer chromatographic methodology has been developed and validated for the concurrent measurement of teneligliptin hydrobromide hydrate and pioglitazone hydrochloride in tablet offering excellent sensitivity, precision, accuracy, and robustness. The methodology involved using aluminum plates layered with silica gel 60F 254 were used, and the solvent system consisted of a mixture of chloroform, methanol, and ammonia (8:1:0.5 v/v/v). The analysis involved scanning of the plate at a wavelength of 229 nm and analyzing the resulting densitograms. The linear correlation was established over a range of concentrations 250–3000 ng/band for teneligliptin hydrobromide hydrate and 187.5–2250 ng/band for pioglitazone hydrochloride. The method displayed detection limits of 21.29 ng/band for teneligliptin hydrobromide hydrate and 25.97 ng/band for pioglitazone hydrochloride. The quantification limits were 64.52 ng/band for teneligliptin hydrobromide hydrate and 78.71 ng/band for pioglitazone hydrochloride. The results of precision parameters showed that the % relative standard deviation of peak area was consistently below 2%, indicating high precision. The accuracy of the method was demonstrated to be between 96% and 103%. Proposed method was found to be superior and capable of overcoming the shortcomings of previously reported methods for the assessment of both the drugs.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-11-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135290753","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}
Abstract An L‐tetrahydropalmatine (L‐THP) imprinted silica gel polymer functionalized with aminated groups was prepared with surface imprinting technique by using L‐THP as template, grafted silica gel as support, methacrylic acid as functional monomer and ethylene glycol dimethyl acrylate as cross‐linker by solution polymerization. The optimum ratio of template, functional monomer, and cross‐linker were found to be 1:4:20 and the conditions of synthesis were 50°C for 18 h. The surface imprinting silica gel polymer of L‐THP was used as a sorbent for L‐THP adsorption and showed better adsorption capacity of L‐THP than that of non‐imprinted polymers. Then the surface imprinting silica gel polymer of L‐THP was filled into the cartridges as the adsorbents of solid‐phase extraction, and the mean recoveries of L‐THP and D‐tetrahydropalmatine were 70.1% and 17.1% with 2.8% and 3.0% of relative standard deviation, respectively.
{"title":"Synthesis and characterization of a surface imprinting silica gel polymer for the resolution of tetrahydropalmatine enantiomers","authors":"Junfang Zhu, Bo Li","doi":"10.1002/sscp.202300136","DOIUrl":"https://doi.org/10.1002/sscp.202300136","url":null,"abstract":"Abstract An L‐tetrahydropalmatine (L‐THP) imprinted silica gel polymer functionalized with aminated groups was prepared with surface imprinting technique by using L‐THP as template, grafted silica gel as support, methacrylic acid as functional monomer and ethylene glycol dimethyl acrylate as cross‐linker by solution polymerization. The optimum ratio of template, functional monomer, and cross‐linker were found to be 1:4:20 and the conditions of synthesis were 50°C for 18 h. The surface imprinting silica gel polymer of L‐THP was used as a sorbent for L‐THP adsorption and showed better adsorption capacity of L‐THP than that of non‐imprinted polymers. Then the surface imprinting silica gel polymer of L‐THP was filled into the cartridges as the adsorbents of solid‐phase extraction, and the mean recoveries of L‐THP and D‐tetrahydropalmatine were 70.1% and 17.1% with 2.8% and 3.0% of relative standard deviation, respectively.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135476111","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}
Mozhgan Khoshsokhan Aziz, Fereshteh Nematollahi, Mohammad Hadi Givianrad
Abstract Formaldehyde (FA) is commonly used in detergents and cosmetics as an antimicrobial and preservative. This substance is toxic to humans and dangerous to health as it causes eye and skin irritation. FA determination is, therefore, a very important quality control parameter. This study developed gas chromatography/mass spectrometry (GC/MS) and solid‐phase microextraction (SPME) with on‐fiber derivatization to determine FA in cosmetic cream skin. FA was derivated using 2,4‐dinitrophenylhydrazine in an aqueous solution. FA in cosmetic cream samples was extracted through SPME fibers in the headspace and rapidly derivated with 2,4‐dinitrophenylhydrazine on SPME fibers. The average detection and quantification limits were at least 0.036 and 0.12, respectively. The results showed that GC/MS and SPME with on‐fiber derivatization are simple, fast, sensitive, and solvent‐free methods for aldehydes determination in cosmetic cream.
{"title":"Determination of formaldehyde in cosmetic creams using gas chromatography/mass spectrometry analysis and solid‐phase microextraction","authors":"Mozhgan Khoshsokhan Aziz, Fereshteh Nematollahi, Mohammad Hadi Givianrad","doi":"10.1002/sscp.202300120","DOIUrl":"https://doi.org/10.1002/sscp.202300120","url":null,"abstract":"Abstract Formaldehyde (FA) is commonly used in detergents and cosmetics as an antimicrobial and preservative. This substance is toxic to humans and dangerous to health as it causes eye and skin irritation. FA determination is, therefore, a very important quality control parameter. This study developed gas chromatography/mass spectrometry (GC/MS) and solid‐phase microextraction (SPME) with on‐fiber derivatization to determine FA in cosmetic cream skin. FA was derivated using 2,4‐dinitrophenylhydrazine in an aqueous solution. FA in cosmetic cream samples was extracted through SPME fibers in the headspace and rapidly derivated with 2,4‐dinitrophenylhydrazine on SPME fibers. The average detection and quantification limits were at least 0.036 and 0.12, respectively. The results showed that GC/MS and SPME with on‐fiber derivatization are simple, fast, sensitive, and solvent‐free methods for aldehydes determination in cosmetic cream.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135479858","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}
Faezeh Zanganeh, Zahra Tayarani‐Najaran, Karel Nesměrák, Martin Štícha, Seyed Ahmad Emami, Maryam Akaberi
Abstract In an ongoing project on the Iranian Helichrysum Mill. species (Asteraceae), the phytochemical profiles of the extracts obtained from the flower and leaves of Helichrysum oligocephalum were investigated utilizing ultra‐performance liquid chromatography–mass spectrometry (MS) coupled with quadrupole time of flight. In addition, the cytotoxic activity of the extracts was evaluated against different cancerous cell lines by AlamarBlue assay. The apoptotic effects of the fractions were measured by propidium iodide staining and flow cytometry. HPLC‐based activity profiling was used to track the cytotoxic constituents. The MS and MS n data were analyzed by MZmine3. Clustering and visualization of the MS data were established by an online platform FreeClust. Concentration‐dependent cytotoxicity was observed for dichloromethane fractions. The active constituents were annotated as pyrone and phloroglucinol derivatives by comparing their MS and MS n profiles to an in‐house library, available databases, Dictionary of Natural Products, and literature. Additionally, plausible MS fragmentation pathways were suggested for the compounds; this can help in the dereplication process of similar compounds from the genus. In conclusion, this plant is rich in valuable phloroglucinol and pyrone compounds and can be used as a source of active phytochemicals. However, further phytochemical and pharmacological studies are necessary.
{"title":"Dereplication of natural cytotoxic products from <i>Helichrysum oligocephalum</i> using ultra‐performance liquid chromatography–quadrupole time of flight‐mass spectrometry","authors":"Faezeh Zanganeh, Zahra Tayarani‐Najaran, Karel Nesměrák, Martin Štícha, Seyed Ahmad Emami, Maryam Akaberi","doi":"10.1002/sscp.202300150","DOIUrl":"https://doi.org/10.1002/sscp.202300150","url":null,"abstract":"Abstract In an ongoing project on the Iranian Helichrysum Mill. species (Asteraceae), the phytochemical profiles of the extracts obtained from the flower and leaves of Helichrysum oligocephalum were investigated utilizing ultra‐performance liquid chromatography–mass spectrometry (MS) coupled with quadrupole time of flight. In addition, the cytotoxic activity of the extracts was evaluated against different cancerous cell lines by AlamarBlue assay. The apoptotic effects of the fractions were measured by propidium iodide staining and flow cytometry. HPLC‐based activity profiling was used to track the cytotoxic constituents. The MS and MS n data were analyzed by MZmine3. Clustering and visualization of the MS data were established by an online platform FreeClust. Concentration‐dependent cytotoxicity was observed for dichloromethane fractions. The active constituents were annotated as pyrone and phloroglucinol derivatives by comparing their MS and MS n profiles to an in‐house library, available databases, Dictionary of Natural Products, and literature. Additionally, plausible MS fragmentation pathways were suggested for the compounds; this can help in the dereplication process of similar compounds from the genus. In conclusion, this plant is rich in valuable phloroglucinol and pyrone compounds and can be used as a source of active phytochemicals. However, further phytochemical and pharmacological studies are necessary.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135479608","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}
Abstract A simple, reliable, and stability‐indicating RP‐HPLC‐UV method was developed and validated for the estimation of related substances ( p ‐chlorophenol and unknown impurities) of chlorzoxazone (skeletal muscle relaxant). Along with this as the compound contains a potential genotoxic impurity (2‐amino‐4‐chlorophenol), which needs to have more sensitivity in quantification, we have also developed and validated a separate RP‐HPLC‐mass spectrometry (MS)/MS method for the estimation of 2‐amino‐4‐chlorophenol impurity. Both methods (RP‐HPLC‐UV & RP‐HPLC–MS/MS) were validated in accordance with International Council for Harmonization Q2(R1) and were found to be precise, accurate, robust, linear, and specific with limit of quantification values established with respect to 100% of test concentration, 0.018% w/w of p ‐chlorophenol by RP‐HPLC‐UV, and 2 ppm of 2‐amino‐4‐chlorophenol by RP‐HPLC–MS.
{"title":"Stability‐indicating method for quantification of potential genotoxic impurity and other organic impurities of chlorzoxazone using hyphenated techniques","authors":"Bhujanga Rao Nagulancha, Vandavasi Koteswara Rao","doi":"10.1002/sscp.202300138","DOIUrl":"https://doi.org/10.1002/sscp.202300138","url":null,"abstract":"Abstract A simple, reliable, and stability‐indicating RP‐HPLC‐UV method was developed and validated for the estimation of related substances ( p ‐chlorophenol and unknown impurities) of chlorzoxazone (skeletal muscle relaxant). Along with this as the compound contains a potential genotoxic impurity (2‐amino‐4‐chlorophenol), which needs to have more sensitivity in quantification, we have also developed and validated a separate RP‐HPLC‐mass spectrometry (MS)/MS method for the estimation of 2‐amino‐4‐chlorophenol impurity. Both methods (RP‐HPLC‐UV & RP‐HPLC–MS/MS) were validated in accordance with International Council for Harmonization Q2(R1) and were found to be precise, accurate, robust, linear, and specific with limit of quantification values established with respect to 100% of test concentration, 0.018% w/w of p ‐chlorophenol by RP‐HPLC‐UV, and 2 ppm of 2‐amino‐4‐chlorophenol by RP‐HPLC–MS.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2023-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"135934563","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}
Ashim Kumar Sen, Satish B Khatariya, Dhanya B Sen, Rajesh A Maheshwari, Ashok H Akabari, Ramaswamy Velmurugan
Abstract Enhanced glycemic regulation in individuals with diabetes mellitus can be achieved using a fixed‐dose combination of dapagliflozin (10 mg) and vildagliptin (100 mg) in tablet. The primary objective of this research was to develop and validate a high‐performance thin layer chromatographic methodology for accurately measuring the quantities of dapagliflozin and vildagliptin in combined tablet formulation. The methodology involved using aluminum plates layered with silica gel 60F 254 , and the solvent system comprised of acetonitrile, benzene, and glacial acetic acid (9:1:2 v/v/v). Densitograms were scanned at a wavelength of 210 nm. The linearity of the procedure was established in the series of 200–2500 ng/band for dapagliflozin and 2000–25000 ng/band for vildagliptin, with correlation coefficients ( r 2 ) of 0.9931 and 0.9954, correspondingly. The method demonstrated good sensitivity, with detection limits of 21.07 ng/band for dapagliflozin and 154.97 ng/band for vildagliptin; quantification limits of 63.84 ng/band for dapagliflozin and 469.60 ng/band for vildagliptin. The methodology was found to be precise (% relative standard deviation of peak area <2) and accurate (recovery between 97% and 103%). Proposed method was found to be superior and capable of overcoming the shortcomings of previously reported methods for the assessment of dapagliflozin and vildagliptin in combined formulation.
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