The determination of Salbutamol and Ketotifen was performed by HPLC and HPTLC methods using 280 nm and 258 nm as the determination wavelength, respectively. Methanol was used to dissolve the drug for estimation in HPLC using mobile phase methanol: 10mM di-Potassium hydrogen orthophosphate in the ratio of 55:45 v/v of pH 4 at a flow rate of 1mL/min and in chloroform: toluene: methanol (7: 2: 3 v/v/v) for the estimation in HPTLC. Moreover, a statistical comparison was made between the results obtained through HPLC and HPTLC of Sal-butamol (SAL) and Ketotifen (KET) using the Student’s t-test and F-test. A linear response was observed in the range of 4-24 μg/mL and 2-12 μg/mL, respective-ly, for SAL and KET for HPLC. R2 was found to be 0.9998 and 0.9999, respectively. For HPTLC, the linear response was observed in the concentration range of 20-120 ng/ spot and 10 - 60 ng/ spot for SAL and KET, respectively. R2 was found to be 0.9988 and 0.9998, respectively. The limit of detection (LOD) for HPLC was estimated as 0.34 μg/ml and 0.10μg/ml for SAL and KET, respectively, and for the HPTLC method, the LOD was estimated as 4.8 μg/ml and 1.5 μg/ml, respectively. Analysing the marketed formulation by using both methods, SAL and KET within the range of 100 ± 2% were recovered. The results obtained after the estimation of the Mastifen S tablet by applying both methods were according to nominal content. Degradation studies were performed using both methods. It was found that Salbutamol was unstable in hydro-lytic, oxidative and thermal degradation, whereas stable in photolytic conditions. Ketotifen was found to be stable in thermal and photolytic conditions and unstable in hydrolytic and oxidative conditions. The proposed stability indicating HPLC and HPTLC methods for SAL and KET was found to be simple, accurate, and reproducible for quantitative estimation in pharmaceutical dos-age form, without interference from the excipients or degradation products from the main drug component.
{"title":"A Statistical-Based Stability-Indicating Assay for the Estimation of Salbutamol and Ketotifen Using HPLC and HPTLC Methods","authors":"Reetu Bandewar, Manik Ghosh, Suddhasattya Dey, Arijit Mondal, Saptarshy Sarkar, Sudip Kumar Mandal, Padma Charan Bahera, Sajal Kumar Jha","doi":"10.2174/0122132406286654240213113940","DOIUrl":"https://doi.org/10.2174/0122132406286654240213113940","url":null,"abstract":"\u0000\u0000The determination of Salbutamol and Ketotifen was performed by HPLC and HPTLC methods using 280 nm and 258 nm as the determination wavelength, respectively. Methanol was used to dissolve the drug for estimation in HPLC using mobile phase methanol: 10mM di-Potassium hydrogen orthophosphate in the ratio of 55:45 v/v of pH 4 at a flow rate of 1mL/min and in chloroform: toluene: methanol (7: 2: 3 v/v/v) for the estimation in HPTLC. Moreover, a statistical comparison was made between the results obtained through HPLC and HPTLC of Sal-butamol (SAL) and Ketotifen (KET) using the Student’s t-test and F-test.\u0000\u0000\u0000\u0000A linear response was observed in the range of 4-24 μg/mL and 2-12 μg/mL, respective-ly, for SAL and KET for HPLC. R2 was found to be 0.9998 and 0.9999, respectively. For HPTLC, the linear response was observed in the concentration range of 20-120 ng/ spot and 10 - 60 ng/ spot for SAL and KET, respectively. R2 was found to be 0.9988 and 0.9998, respectively. The limit of detection (LOD) for HPLC was estimated as 0.34 μg/ml and 0.10μg/ml for SAL and KET, respectively, and for the HPTLC method, the LOD was estimated as 4.8 μg/ml and 1.5 μg/ml, respectively. Analysing the marketed formulation by using both methods, SAL and KET within the range of 100 ± 2% were recovered. The results obtained after the estimation of the Mastifen S tablet by applying both methods were according to nominal content. Degradation studies were performed using both methods. It was found that Salbutamol was unstable in hydro-lytic, oxidative and thermal degradation, whereas stable in photolytic conditions. Ketotifen was found to be stable in thermal and photolytic conditions and unstable in hydrolytic and oxidative conditions.\u0000\u0000\u0000\u0000The proposed stability indicating HPLC and HPTLC methods for SAL and KET was found to be simple, accurate, and reproducible for quantitative estimation in pharmaceutical dos-age form, without interference from the excipients or degradation products from the main drug component.\u0000","PeriodicalId":10826,"journal":{"name":"Current chromatography","volume":"36 9","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-02-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140440655","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}
Standardization of Triphala Juice was performed by using the WHO Guidelines. The Parameters included Preliminary Analysis, Phytochemical Identification, Heavy Metal Estimation, etc. A new simple, specific, precise and accurate UV Spectrophotometric, High-Performance Liquid Methods: Chromatography and High-Performance Thin Layer Chromatography method has been developed for the Estimation of Gallic Acid in pure form. The UV- Spectrophotometric method was developed using Schimadzu 1800 UV - Visible spec-trophotometer using methanol as a solvent. The method was shown to be linear, with a detection wavelength of 273 nm for Gallic Acid. The separation was achieved on the Schimadzu Prominence-I RP-HPLC and the column used was C18 column using mobile phase consisting of mixture of Methanol: 0.1% OPA (50:50). The detection was carried out at 280 nm with a flow rate of 0.7ml/min. The retention time for Gallic Acid was found 3.89 minutes. The calibration curve was found linear (r2 = 0.999) for RP- HPLC method. The HPTLC method was developed using Aetron Sprayline instrument, Methanol as solvent and mobile phase consisting of Toluene: Ethyl Acetate: Formic Acid: Methanol (3:3:0.9:0.2). The method was found linear and the wavelength of detection for Gallic Acid was 254nm, respectively. The percentage recoveries for both methods were found in the 98.0- 102.0% range. The methods were validated in accordance with International Conference on harmoniza-tion acceptance criteria for specificity, linearity, precision, accuracy, robustness and system suita-bility. The excipients did not interfere in the determination of Gallic acid in Triphala Juice. The suggested approach was effectively implemented for the quantitative determina-tion of gallic acid in Triphala juice, which would aid in quality control
{"title":"Standardization and Evaluation of Triphala Juice and Quantification of Gallic Acid as a Biomarker by Analytical Techniques","authors":"Tejas Ahire, Seema Gosavi, Sarita Pawar, Aditi Kulkarni","doi":"10.2174/0122132406260669231214092816","DOIUrl":"https://doi.org/10.2174/0122132406260669231214092816","url":null,"abstract":"\u0000\u0000Standardization of Triphala Juice was performed by using the WHO Guidelines. The Parameters included Preliminary Analysis, Phytochemical Identification, Heavy Metal Estimation, etc.\u0000A new simple, specific, precise and accurate UV Spectrophotometric, High-Performance Liquid Methods: Chromatography and High-Performance Thin Layer Chromatography method has been developed for the Estimation of Gallic Acid in pure form.\u0000The UV- Spectrophotometric method was developed using Schimadzu 1800 UV - Visible spec-trophotometer using methanol as a solvent. The method was shown to be linear, with a detection wavelength of 273 nm for Gallic Acid.\u0000The separation was achieved on the Schimadzu Prominence-I RP-HPLC and the column used was C18 column using mobile phase consisting of mixture of Methanol: 0.1% OPA (50:50). The detection was carried out at 280 nm with a flow rate of 0.7ml/min. The retention time for Gallic Acid was found 3.89 minutes. The calibration curve was found linear (r2 = 0.999) for RP- HPLC method.\u0000The HPTLC method was developed using Aetron Sprayline instrument, Methanol as solvent and mobile phase consisting of Toluene: Ethyl Acetate: Formic Acid: Methanol (3:3:0.9:0.2). The method was found linear and the wavelength of detection for Gallic Acid was 254nm, respectively.\u0000The percentage recoveries for both methods were found in the 98.0- 102.0% range.\u0000\u0000\u0000\u0000The methods were validated in accordance with International Conference on harmoniza-tion acceptance criteria for specificity, linearity, precision, accuracy, robustness and system suita-bility. The excipients did not interfere in the determination of Gallic acid in Triphala Juice.\u0000\u0000\u0000\u0000The suggested approach was effectively implemented for the quantitative determina-tion of gallic acid in Triphala juice, which would aid in quality control\u0000","PeriodicalId":10826,"journal":{"name":"Current chromatography","volume":"118 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-01-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140497256","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 : 2022-11-10DOI: 10.2174/2213240609666221110090339
S. Dubey, Manisha Choudhari, Mahipal Reddy Donthi, S. Damle, Gautam Singhvi, R. Saha
Abiraterone acetate is a derivative of steroidal progesterone, used as a first-line therapy for metastatic castration of prostate cancer. The present study encompasses the design of an experiment approach for developing a simple, reliable, and rapid RP-HPLC method for the estimation of abiraterone acetate. The chromatographic separation was efficiently conducted on a Hypersil Gold C18 (50 x 4.6 mm, 5 µm) HPLC column, using the mobile phase composition of acetonitrile: dibasic potassium phosphate (0.01 mM) in the ratio of 80:20 (%v/v) at pH 6.5 with an isocratic elution mode. Furthermore, the different force degradation study including hydrolysis, oxidation, thermal, and photolytic was performed for abiraterone acetate. The dynamic linearity was established in the concentration range of 0.5-10 µg/mL with r2 of 0.9998. Furthermore, the limit of detection and the limit of quantitation were 0.0978 µg/mL and 0.3260 µg/mL. The degradation of abiraterone acetate was shown in both acidic (54.16 ± 0.247 after 24 hrs) and basic conditions (35.06 ± 0.458 after 24 hrs). Furthermore, the developed method was successfully employed to quantify abiraterone acetate in bulk powder and the solid dispersion did not show any change in the retention time. The developed method was validated according to the ICH Q2 (R1) specification, which was found to be sensitive, accurate, precise, robust, linear, and selective compared to the reported chromatographic method.
{"title":"Implementation of Quality by Design Approach for Optimization of RP-HPLC Method for Quantification of Abiraterone Acetate in Solid Dispersion in Forced Degradation Studies","authors":"S. Dubey, Manisha Choudhari, Mahipal Reddy Donthi, S. Damle, Gautam Singhvi, R. Saha","doi":"10.2174/2213240609666221110090339","DOIUrl":"https://doi.org/10.2174/2213240609666221110090339","url":null,"abstract":"\u0000\u0000Abiraterone acetate is a derivative of steroidal progesterone, used as a first-line therapy for metastatic castration of prostate cancer.\u0000\u0000\u0000\u0000The present study encompasses the design of an experiment approach for developing a simple, reliable, and rapid RP-HPLC method for the estimation of abiraterone acetate.\u0000\u0000\u0000\u0000The chromatographic separation was efficiently conducted on a Hypersil Gold C18 (50 x 4.6 mm, 5 µm) HPLC column, using the mobile phase composition of acetonitrile: dibasic potassium phosphate (0.01 mM) in the ratio of 80:20 (%v/v) at pH 6.5 with an isocratic elution mode. Furthermore, the different force degradation study including hydrolysis, oxidation, thermal, and photolytic was performed for abiraterone acetate.\u0000\u0000\u0000\u0000The dynamic linearity was established in the concentration range of 0.5-10 µg/mL with r2 of 0.9998. Furthermore, the limit of detection and the limit of quantitation were 0.0978 µg/mL and 0.3260 µg/mL. The degradation of abiraterone acetate was shown in both acidic (54.16 ± 0.247 after 24 hrs) and basic conditions (35.06 ± 0.458 after 24 hrs). Furthermore, the developed method was successfully employed to quantify abiraterone acetate in bulk powder and the solid dispersion did not show any change in the retention time.\u0000\u0000\u0000\u0000The developed method was validated according to the ICH Q2 (R1) specification, which was found to be sensitive, accurate, precise, robust, linear, and selective compared to the reported chromatographic method.\u0000","PeriodicalId":10826,"journal":{"name":"Current chromatography","volume":"89 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-11-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85958423","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 : 2022-09-30DOI: 10.2174/2213240609666220930121841
Nikunj Dhirubhai Patel, N. Kanaki
Kutki, the dried rhizome of Picrorhiza kurroa Royle ex Benth belonging to family Scrophulariaceae, has been utilized globally for liver ailments. Comprehensive use of kutki needs to evaluate its role as a quality control tool for discrimination of kutki samples, and therefore an effective HPLC fingerprinting method was established. Reverse-phase high-performance liquid chromatography with photodiode array (RP-HPLC-PDA) detection method coupled with multivariate analysis was developed, which was modest, consistent and, accurate for classification of 11 kutki samples including authentic Picrorhiza kurroa rhizomes from the market of Ahmedabad and Gandhinagar in Gujarat, India. The method was validated for various parameters like precision, reproducibility, and stability. The lowest value of the % relative standard deviations (RSD) was 1.31%. Chromatographic fingerprint profiles of 11 kutki samples, including authenticated samples, were obtained by this method, which showed total 28 peaks, and 9 peaks were important among them. Chemometric techniques like PCA and HCA were applied to identify the kutki samples. Samples of kutki could be exquisitely differentiated into two clusters. HPLC-PDA method coupled to multivariate analysis divulged that chromatographic fingerprint analysis was reliable and effective for quality assessment and discrimination of kutki samples.
{"title":"HPLC Fingerprint Analysis Coupled with Multivariate Analysis for Quality Assesssment of Picrorhiza kurroa rhizomes","authors":"Nikunj Dhirubhai Patel, N. Kanaki","doi":"10.2174/2213240609666220930121841","DOIUrl":"https://doi.org/10.2174/2213240609666220930121841","url":null,"abstract":"\u0000\u0000Kutki, the dried rhizome of Picrorhiza kurroa Royle ex Benth belonging to family Scrophulariaceae, has been utilized globally for liver ailments.\u0000\u0000\u0000\u0000Comprehensive use of kutki needs to evaluate its role as a quality control tool for discrimination of kutki samples, and therefore an effective HPLC fingerprinting method was established.\u0000\u0000\u0000\u0000Reverse-phase high-performance liquid chromatography with photodiode array (RP-HPLC-PDA) detection method coupled with multivariate analysis was developed, which was modest, consistent and, accurate for classification of 11 kutki samples including authentic Picrorhiza kurroa rhizomes from the market of Ahmedabad and Gandhinagar in Gujarat, India.\u0000\u0000\u0000\u0000The method was validated for various parameters like precision, reproducibility, and stability. The lowest value of the % relative standard deviations (RSD) was 1.31%. Chromatographic fingerprint profiles of 11 kutki samples, including authenticated samples, were obtained by this method, which showed total 28 peaks, and 9 peaks were important among them. Chemometric techniques like PCA and HCA were applied to identify the kutki samples. Samples of kutki could be exquisitely differentiated into two clusters.\u0000\u0000\u0000\u0000HPLC-PDA method coupled to multivariate analysis divulged that chromatographic fingerprint analysis was reliable and effective for quality assessment and discrimination of kutki samples.\u0000","PeriodicalId":10826,"journal":{"name":"Current chromatography","volume":"62 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-09-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79678276","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 : 2022-07-28DOI: 10.2174/2213240609666220728091253
Arvind Sharma, F. Ali, A. Prakash, R. K. Goyal
The quality of drugs is a major concern for drug regulatory authorities and other stakeholders across the globe. Recently, drug regulatory authorities across the globe are facing a challenge to control the purity of cardiovascular (CVS) drugs for human use, especially drugs from Angiotensin Receptor Blocker family such as Valsartan. The present article is an attempt to provide a comprehensive knowledge on how pharmacopeias across the world are playing a key role in ensuring the quality of active pharmaceutical ingredients (API) and finished pharmaceutical products (FPPs). The comprehensive information on pharmaceutical impurities, separation strategies, relevant regulatory guidelines to control impurities, and their acceptable limits particularly with respect to cardiovascular active drug substances and drug formulations for human use are focused in this article.
{"title":"Impurities present in cardiovascular active substances and medicinal products: A Pharmacopoeial perspective--","authors":"Arvind Sharma, F. Ali, A. Prakash, R. K. Goyal","doi":"10.2174/2213240609666220728091253","DOIUrl":"https://doi.org/10.2174/2213240609666220728091253","url":null,"abstract":"\u0000\u0000The quality of drugs is a major concern for drug regulatory authorities and other stakeholders across the globe. Recently, drug regulatory authorities across the globe are facing a challenge to control the purity of cardiovascular (CVS) drugs for human use, especially drugs from Angiotensin Receptor Blocker family such as Valsartan. The present article is an attempt to provide a comprehensive knowledge on how pharmacopeias across the world are playing a key role in ensuring the quality of active pharmaceutical ingredients (API) and finished pharmaceutical products (FPPs). The comprehensive information on pharmaceutical impurities, separation strategies, relevant regulatory guidelines to control impurities, and their acceptable limits particularly with respect to cardiovascular active drug substances and drug formulations for human use are focused in this article.\u0000","PeriodicalId":10826,"journal":{"name":"Current chromatography","volume":"92 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-07-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77595886","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 : 2022-03-21DOI: 10.2174/2213240609666220321095729
C. Spagnol, Camila Jandira Martins, A. Kogawa, V. Isaac, H. R. Salgado, M. Correa
A NEW, FAST AND SUSTAINABLE METHOD BY HPLC FOR SIMULTANEOUS DETERMINATION OF ASCORBIC ACID AND NICOTINAMIDE IN COSMETIC EMULSION Nicotinamide (NIC) and ascorbic acid (AA) are powerful antioxidants. AA presents excellent reducing power and protects the cell from oxidation. NIC is a precursor of NADPH and NADH, substances that present a strong reduction power, resulting in a huge antioxidant capacity. A new, fast and sustainable method using high performance liquid chromatography was developed and validated for simultaneous quantification of AA and NIC in cosmetic emulsion. For this, purified water with 0.01 % of trifluoracetic acid and ethanol (95:5, v/v), Symmetry Shield column (4.6 x 250 mm, 5 μm), 20 µL, 1.7 mL min-1 at 254 nm was used. The method was validated according to the ICH, AOAC and ANVISA, following parameters of linearity, detection and quantification limits, selectivity, accuracy, precision and robustness. The method was fast (2.7 min for AA and 3.2 min for NIC), linear between 20 and 80 μg mL-1 (r = 0.9991 for AA and r = 0.9999 for NIC), precise (RSD <5 % for AA and NIC), accuracy (RSD 0.53 % for AA and 1.02 % for NIC), selective for the emulsion base, robust to small changes in flow rate, injection volume and purified water source. This work shows an ecologically alternative for the quantification of AA and NIC in the study of cosmetic emulsion by HPLC, which contemplates the requirements of the current green and sustainable analytical chemistry.
采用高效液相色谱法同时测定化妆品乳剂中抗坏血酸和烟酰胺的含量。烟酰胺和抗坏血酸是强抗氧化剂。AA具有优异的还原能力，保护电池不被氧化。NIC是NADPH和NADH的前体，具有很强的还原能力，具有很强的抗氧化能力。建立了一种快速、可持续的高效液相色谱法同时测定化妆品乳液中AA和NIC的方法。为此，使用含有0.01%三氟乙酸和乙醇(95:5,v/v)的纯净水，对称屏蔽柱(4.6 x 250 mm, 5 μm)， 20µL, 1.7 mL min-1, 254 nm。按照ICH、AOAC和ANVISA标准对该方法进行了线性度、检测定量限、选择性、准确度、精密度和鲁棒性等参数的验证。该方法快速(AA为2.7 min, NIC为3.2 min)，在20 ~ 80 μ mL-1范围内呈线性(AA为0.9991,NIC为r = 0.9999)，精密度(AA和NIC的RSD < 5%)，准确度(AA为0.53%，NIC为1.02%)，对乳状液基质具有选择性，对流速、进样量和纯化水源的微小变化具有较强的适应性。本研究为化妆品乳剂研究中AA和NIC的定量提供了一种生态替代方法，考虑了当前绿色和可持续分析化学的要求。
{"title":"New, fast and sustainable method by hplc for simultaneous determination of ascorbic acid and nicotinamide in the study of cosmetic emulsions","authors":"C. Spagnol, Camila Jandira Martins, A. Kogawa, V. Isaac, H. R. Salgado, M. Correa","doi":"10.2174/2213240609666220321095729","DOIUrl":"https://doi.org/10.2174/2213240609666220321095729","url":null,"abstract":"\u0000\u0000A NEW, FAST AND SUSTAINABLE METHOD BY HPLC FOR SIMULTANEOUS DETERMINATION OF ASCORBIC ACID AND NICOTINAMIDE IN COSMETIC EMULSION\u0000\u0000\u0000\u0000Nicotinamide (NIC) and ascorbic acid (AA) are powerful antioxidants. AA presents excellent reducing power and protects the cell from oxidation. NIC is a precursor of NADPH and NADH, substances that present a strong reduction power, resulting in a huge antioxidant capacity.\u0000\u0000\u0000\u0000A new, fast and sustainable method using high performance liquid chromatography was developed and validated for simultaneous quantification of AA and NIC in cosmetic emulsion.\u0000\u0000\u0000\u0000For this, purified water with 0.01 % of trifluoracetic acid and ethanol (95:5, v/v), Symmetry Shield column (4.6 x 250 mm, 5 μm), 20 µL, 1.7 mL min-1 at 254 nm was used. The method was validated according to the ICH, AOAC and ANVISA, following parameters of linearity, detection and quantification limits, selectivity, accuracy, precision and robustness.\u0000\u0000\u0000\u0000The method was fast (2.7 min for AA and 3.2 min for NIC), linear between 20 and 80 μg mL-1 (r = 0.9991 for AA and r = 0.9999 for NIC), precise (RSD <5 % for AA and NIC), accuracy (RSD 0.53 % for AA and 1.02 % for NIC), selective for the emulsion base, robust to small changes in flow rate, injection volume and purified water source.\u0000\u0000\u0000\u0000This work shows an ecologically alternative for the quantification of AA and NIC in the study of cosmetic emulsion by HPLC, which contemplates the requirements of the current green and sustainable analytical chemistry.\u0000","PeriodicalId":10826,"journal":{"name":"Current chromatography","volume":"31 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-03-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86071429","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 : 2022-03-07DOI: 10.2174/2213240609666220307110010
Shilpa Dawre
The combination of doxycycline (DOXY) and rifampicin (RIF) is recommended as a treatment therapy for brucellosis by the World Health Organization. The aim of the current study was the development and validation of the stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for the analysis of a combination of doxycycline & rifampicin. RP-HPLC method was developed and validated for the estimation of doxycycline and rifampicin combination as per ICH guidelines. The drug combination solution was exposed to different stress conditions viz. acidic, basic, photo-oxidation, and oxidation. The method was found linear in the range of 2 -10μg/mL for both the drugs with a retention time of 3.5 min for doxycycline and 6.5 min for rifampicin at lambda maximum of 350 nm. The RP-HPLC method was found precise and accurate with %RSD < 2%. The intra-day and inter-day precision were calculated and found within the acceptable range of 5%. Both drugs demonstrated good stability in the mobile phase after 6h. The LOD and LOQ of doxycycline and rifampicin were found 100 ng/mL & 200ng/mL and 150ng/mL & 500ng/mL, respectively. The forced degradation of the combination of drug solutions was performed. The degraded drug peaks were well-resolved from the peaks of drugs. The percentage encapsulation efficiency of doxycycline and rifampicin in nanoparticle system was assessed by utilizing the validated RP-HPLC method and found >60% (DOXY) and >70% (RIF). The developed RP-HPLC method of DOXY-RIF combination was rapid, accurate, precise, and stability-indicating. The method can be suitably applied for the determination of drugs in the nanoparticulate system.
{"title":"Development and validation of stability indicating rp-hplc method for simultaneous determination of doxycycline and rifampicin in polymeric nanoparticles","authors":"Shilpa Dawre","doi":"10.2174/2213240609666220307110010","DOIUrl":"https://doi.org/10.2174/2213240609666220307110010","url":null,"abstract":"\u0000\u0000The combination of doxycycline (DOXY) and rifampicin (RIF) is recommended as a treatment therapy for brucellosis by the World Health Organization.\u0000\u0000\u0000\u0000The aim of the current study was the development and validation of the stability-indicating reverse-phase high-performance liquid chromatography (RP-HPLC) method for the analysis of a combination of doxycycline & rifampicin.\u0000\u0000\u0000\u0000RP-HPLC method was developed and validated for the estimation of doxycycline and rifampicin combination as per ICH guidelines. The drug combination solution was exposed to different stress conditions viz. acidic, basic, photo-oxidation, and oxidation.\u0000\u0000\u0000\u0000The method was found linear in the range of 2 -10μg/mL for both the drugs with a retention time of 3.5 min for doxycycline and 6.5 min for rifampicin at lambda maximum of 350 nm. The RP-HPLC method was found precise and accurate with %RSD < 2%. The intra-day and inter-day precision were calculated and found within the acceptable range of 5%. Both drugs demonstrated good stability in the mobile phase after 6h. The LOD and LOQ of doxycycline and rifampicin were found 100 ng/mL & 200ng/mL and 150ng/mL & 500ng/mL, respectively. The forced degradation of the combination of drug solutions was performed. The degraded drug peaks were well-resolved from the peaks of drugs. The percentage encapsulation efficiency of doxycycline and rifampicin in nanoparticle system was assessed by utilizing the validated RP-HPLC method and found >60% (DOXY) and >70% (RIF).\u0000\u0000\u0000\u0000The developed RP-HPLC method of DOXY-RIF combination was rapid, accurate, precise, and stability-indicating. The method can be suitably applied for the determination of drugs in the nanoparticulate system.\u0000","PeriodicalId":10826,"journal":{"name":"Current chromatography","volume":"381 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-03-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86814431","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 : 2022-01-26DOI: 10.2174/2213240609666220126101414
Kerley Cristiane Victorino Romão, F. Fonseca, Fernanda Schindler, Marina Cristina Peres, G. L. da Veiga, E. Pereira, Beatriz da Costa Aguiar Alves
The 6-mercaptopurine is an active ingredient used to treat certain types of leukemia. This drug is an immunosuppressive and antineoplastic agent that belongs to the thiopurine class. In Brazil, 6-MP is currently available only in the form of 50 mg tablets, sold as Purinethol® and manufactured by Glaxo Smith Kline. The lack of the liquid formulation’s production impedes treatment, assuming that one of its advantages go through its applicability in pediatric patients, which shows the highest incidence among others. The purpose of this work was to evaluate the development and application of a reverse phase high performance liquid chromatography (HPLC) method using an Agilent 1220 Infinity® G4294B chromatograph with photodiode array detector. HPLC assays were performed on an Eclipse plus® C18 column (4.6 x 150 mm, 3.5 µm particle size) using a gradient mode mixture of acetonitrile and aqueous acetic acid solution as a mobile phase, with a flow of 1 mL.min-1 and detection at 324 nm. The method was validated by determining its selectivity, linearity, precision, accuracy, and robustness. Retention time for 6-mercaptopurine was 5.12 minutes. The detector’s response was linear at concentrations from 1.6 to 2.4 µg/mL. The results of the method’s accuracy evaluation of the accuracy showed with mean recovery of the amount of substance added to the samples of between 99.88 and 100.5%. For precision, repeatability and intermediate precision were evaluated. The repeatability showed standard deviation of 0.0737. The intermediate precision was assessed on three different. For the three days of the studies, the values of the standard deviations were less than 3%, showing repeatability and intermediate precision adequate for the analytical method in question. The limit of detection was determined as 3.6 ng/mL. The limit of quantification was determined as 12 ng/mL. The chromatographic method was robust under the proposed The proposed method can be applied to quality control of 6-MP oral suspension to ensure that the required content is delivered to pediatric oncology patients.
6-巯基嘌呤是一种用于治疗某些类型白血病的活性成分。该药是一种免疫抑制和抗肿瘤药物，属于硫嘌呤类。在巴西，6-MP目前仅以50毫克片剂的形式出售，名为Purinethol®，由葛兰素史克(Glaxo Smith Kline)生产。缺乏液体配方的生产阻碍了治疗，假设它的优势之一是它在儿科患者中的适用性，这在其他患者中发病率最高。本研究的目的是评估使用安捷伦1220 Infinity®G4294B光电二极管阵列检测器的反相高效液相色谱(HPLC)方法的开发和应用。HPLC检测采用Eclipse plus®C18色谱柱(4.6 x 150 mm, 3.5µm粒径)，流动相为乙腈和乙酸水溶液的梯度模式混合物，流速为1 mL.min-1，检测波长为324 nm。通过对该方法的选择性、线性度、精密度、准确度和鲁棒性进行验证。6-巯基嘌呤保留时间为5.12 min。在1.6 ~ 2.4µg/mL浓度范围内，检测器的响应呈线性。准确度评价结果表明，该方法的平均加样回收率在99.88 ~ 100.5%之间。对精密度、重复性和中间精密度进行了评价。重复性标准偏差为0.0737。对三种不同的中间精度进行了评估。在为期三天的研究中，标准偏差值小于3%，显示出可重复性和中等精度足以用于所讨论的分析方法。检出限为3.6 ng/mL。定量限为12 ng/mL。该方法可用于6-MP口服混悬液的质量控制，以确保所需的含量被送到儿科肿瘤患者的体内。
{"title":"Development and validation of a HPLC analytical method to determine 6-merpactopurine concentration in oral suspension","authors":"Kerley Cristiane Victorino Romão, F. Fonseca, Fernanda Schindler, Marina Cristina Peres, G. L. da Veiga, E. Pereira, Beatriz da Costa Aguiar Alves","doi":"10.2174/2213240609666220126101414","DOIUrl":"https://doi.org/10.2174/2213240609666220126101414","url":null,"abstract":"\u0000\u0000The 6-mercaptopurine is an active ingredient used to treat certain types of leukemia. This drug is an immunosuppressive and antineoplastic agent that belongs to the thiopurine class. In Brazil, 6-MP is currently available only in the form of 50 mg tablets, sold as Purinethol® and manufactured by Glaxo Smith Kline. The lack of the liquid formulation’s production impedes treatment, assuming that one of its advantages go through its applicability in pediatric patients, which shows the highest incidence among others.\u0000\u0000\u0000\u0000The purpose of this work was to evaluate the development and application of a reverse phase high performance liquid chromatography (HPLC) method using an Agilent 1220 Infinity® G4294B chromatograph with photodiode array detector.\u0000\u0000\u0000\u0000HPLC assays were performed on an Eclipse plus® C18 column (4.6 x 150 mm, 3.5 µm particle size) using a gradient mode mixture of acetonitrile and aqueous acetic acid solution as a mobile phase, with a flow of 1 mL.min-1 and detection at 324 nm. The method was validated by determining its selectivity, linearity, precision, accuracy, and robustness.\u0000\u0000\u0000\u0000Retention time for 6-mercaptopurine was 5.12 minutes. The detector’s response was linear at concentrations from 1.6 to 2.4 µg/mL. The results of the method’s accuracy evaluation of the accuracy showed with mean recovery of the amount of substance added to the samples of between 99.88 and 100.5%. For precision, repeatability and intermediate precision were evaluated. The repeatability showed standard deviation of 0.0737. The intermediate precision was assessed on three different. For the three days of the studies, the values of the standard deviations were less than 3%, showing repeatability and intermediate precision adequate for the analytical method in question. The limit of detection was determined as 3.6 ng/mL. The limit of quantification was determined as 12 ng/mL. The chromatographic method was robust under the proposed\u0000\u0000\u0000\u0000The proposed method can be applied to quality control of 6-MP oral suspension to ensure that the required content is delivered to pediatric oncology patients.\u0000","PeriodicalId":10826,"journal":{"name":"Current chromatography","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-01-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84914252","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 : 2022-01-20DOI: 10.2174/2213240609666220120113938
V. P. Pchelkin
Analysis of experimental retention data upon several variants of argentation liquid chromatographic separations of different mixtures of the same lipid class into their molecular species was made to estimate new parameters of their π-complexes for every unsaturated fatty acid residue as its silver ion cluster. Planar reversed-phase liquid chromatography both in the presence and in the absence of silver ions as well as adsorption argentation liquid chromatography were applied for the separation of complex rac-1,2-diacylglycerol samples from three plant sources (cocoa butter, poppy seed, and linseed oils). Every value of the argentation liquid chromatographic separation selectivity for any lipid molecular species upon both planar and column variants of reversed-phase fractionation of different complex samples from native sources into their molecular components is described by additive relative polarity levels of their fatty acid residues. These levels are always connected with equivalent lipophilicity values for every lipid molecule and its chemical potential variations during all variants of reversed-phase liquid chromatography in the presence of silver ion clusters. New parameters for several fatty acid residues of major native polyunsaturated lipid samples may be reflected by different coordination numbers of single silver atoms of its triangular pyramidal nanoclusters. Both hydrophobicity and total polarity levels of the coordination complexes of different lipid molecular species upon their adsorption argentation liquid chromatography may be also quantitatively estimated by their fixed methylene unit variations of these molecular species for two centigrade lipid scales.
{"title":"A quantitative estimation of the behaviour of unsaturated lipid molecular species during their argentation liquid chromatographic separation","authors":"V. P. Pchelkin","doi":"10.2174/2213240609666220120113938","DOIUrl":"https://doi.org/10.2174/2213240609666220120113938","url":null,"abstract":"\u0000\u0000Analysis of experimental retention data upon several variants of argentation liquid chromatographic separations of different mixtures of the same lipid class into their molecular species was made to estimate new parameters of their π-complexes for every unsaturated fatty acid residue as its silver ion cluster.\u0000\u0000\u0000\u0000Planar reversed-phase liquid chromatography both in the presence and in the absence of silver ions as well as adsorption argentation liquid chromatography were applied for the separation of complex rac-1,2-diacylglycerol samples from three plant sources (cocoa butter, poppy seed, and linseed oils).\u0000\u0000\u0000\u0000Every value of the argentation liquid chromatographic separation selectivity for any lipid molecular species upon both planar and column variants of reversed-phase fractionation of different complex samples from native sources into their molecular components is described by additive relative polarity levels of their fatty acid residues. These levels are always connected with equivalent lipophilicity values for every lipid molecule and its chemical potential variations during all variants of reversed-phase liquid chromatography in the presence of silver ion clusters.\u0000\u0000\u0000\u0000New parameters for several fatty acid residues of major native polyunsaturated lipid samples may be reflected by different coordination numbers of single silver atoms of its triangular pyramidal nanoclusters. Both hydrophobicity and total polarity levels of the coordination complexes of different lipid molecular species upon their adsorption argentation liquid chromatography may be also quantitatively estimated by their fixed methylene unit variations of these molecular species for two centigrade lipid scales.\u0000","PeriodicalId":10826,"journal":{"name":"Current chromatography","volume":"38 10 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-01-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82819921","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 : 2021-12-02DOI: 10.2174/2213240608666211202092036
D. Diab, K. Sridharan
This study aimed to develop a high-performance liquid chromatography (HPLC) technique for estimating paracetamol glucuronide and paracetamol sulphate in the urine samples of preterm neonates. Validated methods exist for estimating the principal metabolites of paracetamol in older children and those with liver disease. Here, we have developed and validated a simple technique for estimating the same in urine samples of preterm neonates. The study aims to develop and validate a simple, reliable, and accurate HPLC technique for estimating urinary paracetamol glucuronide and paracetamol sulphate metabolites. Preterm neonates of either sex diagnosed with patent ductus arteriosus (PDA) receiving paracetamol intravenously at the dose of 15 mg/kg every six hours were recruited. We ran the samples under standardized chromatographic conditions and using various dilutions of the calibration standards. Measures of assay selectivity, linearity, accuracy, and precision were estimated. We observed that the peaks for paracetamol glucuronide and paracetamol sulphate were distinguished from those of the drug-free urine samples. The results for both metabolites revealed good reproducibility, with a percent coefficient of variation (% CV) of 4.3 and 4.9 for the slope for paracetamol glucuronide and paracetamol sulphate, respectively. Similarly, we observed good linearity, as indicated by the correlation coefficients of 0.99 for the metabolites. The validation assays revealed that the method is linear, accurate, and precise over the defined concentration ranges. We demonstrated that HPLC has good accuracy, reliability, and precision, and it can be used for estimating the principal metabolites from urine samples in neonates for defining the ontogeny of conjugation enzymes and in paracetamol overdose.
{"title":"Development of urinary assay methods for estimation of paracetamol glucuronide and paracetamol sulphate in preterm neonates with patent ductus arteriosus.","authors":"D. Diab, K. Sridharan","doi":"10.2174/2213240608666211202092036","DOIUrl":"https://doi.org/10.2174/2213240608666211202092036","url":null,"abstract":"\u0000\u0000\u0000This study aimed to develop a high-performance liquid chromatography (HPLC) technique for estimating paracetamol glucuronide and paracetamol sulphate in the urine samples of preterm neonates.\u0000\u0000\u0000\u0000\u0000Validated methods exist for estimating the principal metabolites of paracetamol in older children and those with liver disease. Here, we have developed and validated a simple technique for estimating the same in urine samples of preterm neonates.\u0000\u0000\u0000\u0000\u0000The study aims to develop and validate a simple, reliable, and accurate HPLC technique for estimating urinary paracetamol glucuronide and paracetamol sulphate metabolites. \u0000\u0000\u0000\u0000\u0000Preterm neonates of either sex diagnosed with patent ductus arteriosus (PDA) receiving paracetamol intravenously at the dose of 15 mg/kg every six hours were recruited. We ran the samples under standardized chromatographic conditions and using various dilutions of the calibration standards. Measures of assay selectivity, linearity, accuracy, and precision were estimated.\u0000\u0000\u0000\u0000\u0000We observed that the peaks for paracetamol glucuronide and paracetamol sulphate were distinguished from those of the drug-free urine samples. The results for both metabolites revealed good reproducibility, with a percent coefficient of variation (% CV) of 4.3 and 4.9 for the slope for paracetamol glucuronide and paracetamol sulphate, respectively. Similarly, we observed good linearity, as indicated by the correlation coefficients of 0.99 for the metabolites. The validation assays revealed that the method is linear, accurate, and precise over the defined concentration ranges.\u0000\u0000\u0000\u0000\u0000We demonstrated that HPLC has good accuracy, reliability, and precision, and it can be used for estimating the principal metabolites from urine samples in neonates for defining the ontogeny of conjugation enzymes and in paracetamol overdose. \u0000\u0000","PeriodicalId":10826,"journal":{"name":"Current chromatography","volume":"8 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2021-12-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79496337","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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