Karthik Rajendran, B. K. Chekraverthy, R. Peraman, Hem Kumar, Rajendran Sankham Devendran, Bruhan Kaggwa, K. Nagappan
Spironolactone is one of the non‐selective mineralocorticoid receptor antagonists acting as anti‐diuretic drugs. Spironolactone is reported to possess mild to severe hyperkalemia which could often result in fatal conditions. Although several analytical methods for evaluating spironolactone as tablet dosage forms have been established in human biological systems, it is crucial to highlight that these approaches are still limited to the suspension dosage form. In this study, we have quantified spironolactone suspension in human plasma with an efficient, sensitive, and optimized ultra‐performance liquid chromatography (UPLC)‐tandem mass spectrometry‐based bioanalytical method using a deuterated internal standard method. A reverse phase UPLC analysis and mass spectrometric detection was performed using electrospray ionization in positive ion mode as an interface, and multiple reaction monitoring as a mode of acquisition. The retention of Spironolactone (SL) and Spironolactone d7 (SL‐d7) was found to be around 6.15 and 6.07 min, respectively. The linearity range was 1.007–100.224 ng/mL for SL with 0.1 mL sample volume. The method was successfully applied to the pharmacokinetic study of spironolactone in healthy male volunteers by administrating 25 mg/5 mL oral suspension and is in accordance with bioanalytical guidelines.
{"title":"Biochemical assessment of spironolactone oral suspension in human plasma using ultra‐performance liquid chromatography‐tandem mass spectrometry: Application toward pharmacokinetic study","authors":"Karthik Rajendran, B. K. Chekraverthy, R. Peraman, Hem Kumar, Rajendran Sankham Devendran, Bruhan Kaggwa, K. Nagappan","doi":"10.1002/sscp.202300174","DOIUrl":"https://doi.org/10.1002/sscp.202300174","url":null,"abstract":"Spironolactone is one of the non‐selective mineralocorticoid receptor antagonists acting as anti‐diuretic drugs. Spironolactone is reported to possess mild to severe hyperkalemia which could often result in fatal conditions. Although several analytical methods for evaluating spironolactone as tablet dosage forms have been established in human biological systems, it is crucial to highlight that these approaches are still limited to the suspension dosage form. In this study, we have quantified spironolactone suspension in human plasma with an efficient, sensitive, and optimized ultra‐performance liquid chromatography (UPLC)‐tandem mass spectrometry‐based bioanalytical method using a deuterated internal standard method. A reverse phase UPLC analysis and mass spectrometric detection was performed using electrospray ionization in positive ion mode as an interface, and multiple reaction monitoring as a mode of acquisition. The retention of Spironolactone (SL) and Spironolactone d7 (SL‐d7) was found to be around 6.15 and 6.07 min, respectively. The linearity range was 1.007–100.224 ng/mL for SL with 0.1 mL sample volume. The method was successfully applied to the pharmacokinetic study of spironolactone in healthy male volunteers by administrating 25 mg/5 mL oral suspension and is in accordance with bioanalytical guidelines.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-01-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139389349","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}
This study presents a new and rapid analytical high‐performance liquid chromatography coupled with a photodiode array detector method for determining nickel ion (Ni2+) complex with Schiff base (Z)‐1‐(thiophen‐2‐yl‐methyleneamino) propane‐2‐ol easily. The influence of pH, surfactant, and effect of mobile phase on the formation of the Ni‐(Z)‐1‐(thiophen‐2‐yl‐methyleneamino)propane‐2‐ol complex was studied and optimized. The results showed that the acidic condition (pH = 5) favors the complexation most. Triton X‐100 neutral surfactant was used for dissolving the Ni–complex synthesized. A mobile phase ratio of methanol:acetonitrile:water 70:20:10, v/v/v was taken as optimum. This approach allowed the analysis of Ni2+ ion with the limit of detection of 0.0349 ng/mL over the linear range of (0.1–250 ng/mL) and a relative standard deviation of < 2%. The developed method exhibited remarkable extraction recoveries for Ni2+ in various real water samples (tap water; 98.0%–99.8% and river water; 97.0%–98.7%) and alloys with recoveries of (nichrome; 85.2% and chromel; 88.4%). Moreover, this protocol was also applied for the quantitation of Ni2+ in real sewage samples at a concentration level of 0.256 ng/mL. The outcomes of the present work successfully revealed the apparent superiority of Schiff base (Z)‐1‐(thiophen‐2‐yl‐methyleneamino) propane‐2‐ol toward the practical removal of target Ni2+ under real‐world conditions.
{"title":"An approach to determine nickel in aqueous systems through complexation with a Schiff base based on high‐performance liquid chromatography coupled with photodiode array detector","authors":"Asnake Lealem Birhanu, Irshad Mohiuddin","doi":"10.1002/sscp.202300098","DOIUrl":"https://doi.org/10.1002/sscp.202300098","url":null,"abstract":"This study presents a new and rapid analytical high‐performance liquid chromatography coupled with a photodiode array detector method for determining nickel ion (Ni2+) complex with Schiff base (Z)‐1‐(thiophen‐2‐yl‐methyleneamino) propane‐2‐ol easily. The influence of pH, surfactant, and effect of mobile phase on the formation of the Ni‐(Z)‐1‐(thiophen‐2‐yl‐methyleneamino)propane‐2‐ol complex was studied and optimized. The results showed that the acidic condition (pH = 5) favors the complexation most. Triton X‐100 neutral surfactant was used for dissolving the Ni–complex synthesized. A mobile phase ratio of methanol:acetonitrile:water 70:20:10, v/v/v was taken as optimum. This approach allowed the analysis of Ni2+ ion with the limit of detection of 0.0349 ng/mL over the linear range of (0.1–250 ng/mL) and a relative standard deviation of < 2%. The developed method exhibited remarkable extraction recoveries for Ni2+ in various real water samples (tap water; 98.0%–99.8% and river water; 97.0%–98.7%) and alloys with recoveries of (nichrome; 85.2% and chromel; 88.4%). Moreover, this protocol was also applied for the quantitation of Ni2+ in real sewage samples at a concentration level of 0.256 ng/mL. The outcomes of the present work successfully revealed the apparent superiority of Schiff base (Z)‐1‐(thiophen‐2‐yl‐methyleneamino) propane‐2‐ol toward the practical removal of target Ni2+ under real‐world conditions.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-01-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139387943","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}
Celastrus paniculatus, a medicinal plant with diverse therapeutic activities, is known as ‘malkangani’ in the traditional medicine system of India, Ayurveda. It is well known for its memory‐enhancing potential. The reported work involves the gas chromatography‐mass spectrophotometric analysis of cold‐pressed seed oil of Celastrus paniculatus. It revealed the presence of components such as monosaturated fatty acids, polyunsaturated long‐chain fatty acids, and their derivatives. It also showed the presence of terpenes such as squalene, β amyrone, β amyrin acetate, and long‐chain hydrocarbons. Among all the constituents, squalene was found to be a major component. Hence, considering the potential pharmacological actions of squalene, a high‐performance thin‐layer chromatographic (HPTLC) method has been developed for its quantification and subsequently validated as per the International Conference of Harmonization guidelines. A HPTLC fingerprint of oil was obtained on pre‐coated silica gel 60 F254 aluminum sheets, using n‐hexane‐diethyl ether‐glacial acetic acid (7:3:0.05 v/v/v). A densitometric scan was performed at 470 nm after derivatization with vanillin sulphuric acid to quantify squalene. A well‐resolved squalene peak was obtained at a retardation factor of 0.85. It is a simple approach for the estimation of squalene in Celastrus paniculatus seed oil for quality control.
{"title":"Gas chromatography‐mass spectrophotometric profile of cold‐pressed Celastrus paniculatus seed oil and its high‐performance thin‐layer chromatographic analysis emphasizing squalene content","authors":"Suvarna Jarande, Mrinalini Damle","doi":"10.1002/sscp.202300179","DOIUrl":"https://doi.org/10.1002/sscp.202300179","url":null,"abstract":"Celastrus paniculatus, a medicinal plant with diverse therapeutic activities, is known as ‘malkangani’ in the traditional medicine system of India, Ayurveda. It is well known for its memory‐enhancing potential. The reported work involves the gas chromatography‐mass spectrophotometric analysis of cold‐pressed seed oil of Celastrus paniculatus. It revealed the presence of components such as monosaturated fatty acids, polyunsaturated long‐chain fatty acids, and their derivatives. It also showed the presence of terpenes such as squalene, β amyrone, β amyrin acetate, and long‐chain hydrocarbons. Among all the constituents, squalene was found to be a major component. Hence, considering the potential pharmacological actions of squalene, a high‐performance thin‐layer chromatographic (HPTLC) method has been developed for its quantification and subsequently validated as per the International Conference of Harmonization guidelines. A HPTLC fingerprint of oil was obtained on pre‐coated silica gel 60 F254 aluminum sheets, using n‐hexane‐diethyl ether‐glacial acetic acid (7:3:0.05 v/v/v). A densitometric scan was performed at 470 nm after derivatization with vanillin sulphuric acid to quantify squalene. A well‐resolved squalene peak was obtained at a retardation factor of 0.85. It is a simple approach for the estimation of squalene in Celastrus paniculatus seed oil for quality control.","PeriodicalId":508518,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-01-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"139452152","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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