Ai-Lian Zhang, Hanqi Zhang, Xianqin Wang, Shuangqian Chen, Yongxi Jin
In this study, a UPLC-MS/MS method was developed for determination of pancratistatin in the mouse blood, and the pharmacokinetics of pancratistatin in mice after intravenous (5 mg kg−1) and intragastric (15 mg kg−1) administration was studied. HSS T3 column was used for separation with mobile phases of acetonitrile and 0.1% formic acid using gradient elution procedure. The blood sample was treated by protein precipitant with acetonitrile, midazolam was used as internal standard (IS). Multiple reaction monitoring mode (MRM) was used for quantitative analysis, m/z 326.2→83.8 for pancratistatin and m/z 326.2→291.4 for IS in electrospray (ESI) positive interface. It showed a good linear in the range of 10–4,000 ng mL−1 (r > 0.998); the intra-day and inter-day precision was <15%, and the accuracy was 93%–105%. The recovery was better than 82%, and the matrix effect was 94%–105%. The developed UPLC-MS/MS method was fast, selective, and suitable for the pharmacokinetics of pancratistatin in mice.
在本研究中，建立了一种UPLC-MS/MS方法来测定小鼠血液中的胰蛋白酶抑制剂，以及静脉注射后胰蛋白酶抑制剂在小鼠体内的药代动力学（5 mg kg−1）和胃内（15 mg kg−1）给药。采用HSS T3柱，以乙腈和0.1%甲酸为流动相，梯度洗脱。血液样品用蛋白质沉淀剂和乙腈处理，咪达唑仑作为内标（IS）。多反应监测模式（MRM）用于定量分析，m/z 326.2→胰蛋白酶抑制剂83.8和m/z 326.2→291.4用于电喷雾（ESI）正界面中的IS。它在10-4000范围内显示出良好的线性 ng mL−1（r＞0.998）；日间和日间精密度<15%，准确度为93%-105%。回收率优于82%，基质效应为94%-105%。所开发的UPLC-MS/MS方法快速、选择性强，适用于pancratistatin在小鼠体内的药代动力学。
{"title":"Determination of pancratistatin in mouse blood by ultra-liquid chromatography-tandem quadrupole mass spectrometry and its application","authors":"Ai-Lian Zhang, Hanqi Zhang, Xianqin Wang, Shuangqian Chen, Yongxi Jin","doi":"10.1556/1326.2023.01114","DOIUrl":"https://doi.org/10.1556/1326.2023.01114","url":null,"abstract":"In this study, a UPLC-MS/MS method was developed for determination of pancratistatin in the mouse blood, and the pharmacokinetics of pancratistatin in mice after intravenous (5 mg kg−1) and intragastric (15 mg kg−1) administration was studied. HSS T3 column was used for separation with mobile phases of acetonitrile and 0.1% formic acid using gradient elution procedure. The blood sample was treated by protein precipitant with acetonitrile, midazolam was used as internal standard (IS). Multiple reaction monitoring mode (MRM) was used for quantitative analysis, m/z 326.2→83.8 for pancratistatin and m/z 326.2→291.4 for IS in electrospray (ESI) positive interface. It showed a good linear in the range of 10–4,000 ng mL−1 (r > 0.998); the intra-day and inter-day precision was <15%, and the accuracy was 93%–105%. The recovery was better than 82%, and the matrix effect was 94%–105%. The developed UPLC-MS/MS method was fast, selective, and suitable for the pharmacokinetics of pancratistatin in mice.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-03-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43782251","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A rapid and simple method for the determination of stearic acid and 12-hydroxystearic acid in PEG-60 hydrogenated castor oil by high performance liquid chromatography with evaporative light scattering detection was established. The oil sample was first pretreated by alkaline hydrolysis. The analysis was performed on a Zhongpu Develop XD-C18 column (250 mm × 4.6 mm, 5 µm) with gradient elution of methanol and 1% acetic acid aqueous solution at a flow rate of 1.2 mL·min−1 and a column temperature of 40 °C. The drift tube temperature of the evaporative light scattering detection system was set at 40 °C, and the pressure of carrier gas (N2) was 337 kPa. The regression equation revealed a good linear relation (r = 0.9993–0.9995) during the test ranges (119.1–1190.7 μg·mL−1 for 12-hydroxystearic acid, 10.7–107.4 μg·mL−1 for stearic acid). The detection limits of 12-hydroxystearic acid and stearic acid were 1.1 and 2.5 μg·mL−1, the limits of quantitation were 3.2 and 7.4 μg·mL−1, respectively. And the mean recoveries were 101.5 and 101.0%, the corresponding relative standard deviations (RSDs) were 2.1 and 2.8%, respectively. The RSDs corresponding to repeatability (n = 6) were both less than 1.7% in terms of precision. As to the stability, the test results remained stable after 8 h at room temperature (RSDs were both less than 2.6%). The developed method showed high sensitivity, recovery, repeatability and stability, which indicated that the method could be applied as a quality evaluation method for the determination of stearic acid and 12-hydroxyoctadecanoic acid in PEG-60 hydrogenated castor oil.
{"title":"Determination of stearic acid and 12-hydroxyoctadecanoic acid in PEG-60 hydrogenated castor oil by HPLC-ELSD after alkaline hydrolysis","authors":"Yu Duan, Xian-Zhao Liu, En-Nian Li, Zhong-Jing Guo, Xinjun Xu","doi":"10.1556/1326.2023.01116","DOIUrl":"https://doi.org/10.1556/1326.2023.01116","url":null,"abstract":"A rapid and simple method for the determination of stearic acid and 12-hydroxystearic acid in PEG-60 hydrogenated castor oil by high performance liquid chromatography with evaporative light scattering detection was established. The oil sample was first pretreated by alkaline hydrolysis. The analysis was performed on a Zhongpu Develop XD-C18 column (250 mm × 4.6 mm, 5 µm) with gradient elution of methanol and 1% acetic acid aqueous solution at a flow rate of 1.2 mL·min−1 and a column temperature of 40 °C. The drift tube temperature of the evaporative light scattering detection system was set at 40 °C, and the pressure of carrier gas (N2) was 337 kPa. The regression equation revealed a good linear relation (r = 0.9993–0.9995) during the test ranges (119.1–1190.7 μg·mL−1 for 12-hydroxystearic acid, 10.7–107.4 μg·mL−1 for stearic acid). The detection limits of 12-hydroxystearic acid and stearic acid were 1.1 and 2.5 μg·mL−1, the limits of quantitation were 3.2 and 7.4 μg·mL−1, respectively. And the mean recoveries were 101.5 and 101.0%, the corresponding relative standard deviations (RSDs) were 2.1 and 2.8%, respectively. The RSDs corresponding to repeatability (n = 6) were both less than 1.7% in terms of precision. As to the stability, the test results remained stable after 8 h at room temperature (RSDs were both less than 2.6%). The developed method showed high sensitivity, recovery, repeatability and stability, which indicated that the method could be applied as a quality evaluation method for the determination of stearic acid and 12-hydroxyoctadecanoic acid in PEG-60 hydrogenated castor oil.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-03-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49296346","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Indapamide (Indp) and certain other diuretics have been abused in sports, therefore, having sensitive methods for its detection and assay in biological fluids (whole blood, plasma, serum, and urine) is of significant importance. The racemic mixture of Indp is being used as an active pharmaceutical ingredient among other commonly prescribed diuretics. The regulatory authorities and pharmaceutical industries demand analytical methods for successful enantioseparation of such molecules. The paper presents a critical overview of the scientific issues of the application of contemporary techniques involving various chromatographic approaches (with liquid or supercritical fluid as mobile phases) and capillary electrophoresis and method development, for drug screening, assay, bioequivalence studies and enantioseparation of indapamide with their results. It also covers the historical developments that led to significant breakthroughs in research and concise evaluations of research in the area.Different types of chromatographic methods (HPLC, CEC, SFC etc) discussed herein provide an insight and a choice to select a method to (i) screen Indp for drug abuse, (ii) separate, isolate and quantify the enantiomers of Indp and (iii) investigate their pharmacokinetics as markedly different species and not as a total drug. The article evaluates the field's status with a broad base and practical oriented approach so that the underlying principles are easily understood to help chemists and non-specialists gain useful insights into the field outside their specialization and provide experts with summaries of key developments. To the best of authors' knowledge there has been no attempt to review such methods for analysis of Indp and this is the first report of its kind.
{"title":"Chromatographic methods and approaches for bioequivalence study, drug screening and enantioseparation of indapamide","authors":"Sonika Sethi, J. Martens, R. Bhushan","doi":"10.1556/1326.2023.01123","DOIUrl":"https://doi.org/10.1556/1326.2023.01123","url":null,"abstract":"Indapamide (Indp) and certain other diuretics have been abused in sports, therefore, having sensitive methods for its detection and assay in biological fluids (whole blood, plasma, serum, and urine) is of significant importance. The racemic mixture of Indp is being used as an active pharmaceutical ingredient among other commonly prescribed diuretics. The regulatory authorities and pharmaceutical industries demand analytical methods for successful enantioseparation of such molecules. The paper presents a critical overview of the scientific issues of the application of contemporary techniques involving various chromatographic approaches (with liquid or supercritical fluid as mobile phases) and capillary electrophoresis and method development, for drug screening, assay, bioequivalence studies and enantioseparation of indapamide with their results. It also covers the historical developments that led to significant breakthroughs in research and concise evaluations of research in the area.Different types of chromatographic methods (HPLC, CEC, SFC etc) discussed herein provide an insight and a choice to select a method to (i) screen Indp for drug abuse, (ii) separate, isolate and quantify the enantiomers of Indp and (iii) investigate their pharmacokinetics as markedly different species and not as a total drug. The article evaluates the field's status with a broad base and practical oriented approach so that the underlying principles are easily understood to help chemists and non-specialists gain useful insights into the field outside their specialization and provide experts with summaries of key developments. To the best of authors' knowledge there has been no attempt to review such methods for analysis of Indp and this is the first report of its kind.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-02-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48047705","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
M. Antunovic, Jelena Džudović, V. Kilibarda, S. Vučinić, Snezana Djordjevic
Pregabalin is a gabapentinoid approved for the treatment of general anxiety disorder, neuropathic pain and as adjunctive therapy for focal seizures in patients with epilepsy. In addition, there are a number of conditions for which pregabalin is prescribed off-label. Along with the widespread use there are a significant number of reports describing the misuse of pregabalin over the last decade. Over time, it became clear that pregabalin should become part of routine testing in toxicology laboratories. The aim of this paper was to present validation of a LC-MS/MS method for the quantification of pregabalin in plasma of acutely poisoned patients. Simple sample preparation step and rapid chromatographic separation shortened the overall analysis time, which was the goal of method development. The presence of pregabalin was confirmed with three ion transitions, ensuring high selectivity of the validated method. The statistical data obtained showed good precision and accuracy over a wide concentration range. No endogenous or other interference was detected, and there was no matrix effect influence with this method. The LC-MS/MS method was applied to quantify pregabalin in plasma samples of patients admitted to the emergency department due to a possible acute pregabalin overdose. Different concentrations were found, and we report, to the best of our knowledge, the highest plasma concentration of pregabalin in the plasma of a patient with acute poisoning. In conclusion, we developed a fast and simple LC-MS/MS method for reliable determination of pregabalin and demonstrated the developed method was suitable for routine use in clinical toxicology setting.
{"title":"Validation of the rapid and simple LC-MS/MS method for the quantification of pregabalin in plasma of acutely poisoned patients","authors":"M. Antunovic, Jelena Džudović, V. Kilibarda, S. Vučinić, Snezana Djordjevic","doi":"10.1556/1326.2023.01104","DOIUrl":"https://doi.org/10.1556/1326.2023.01104","url":null,"abstract":"Pregabalin is a gabapentinoid approved for the treatment of general anxiety disorder, neuropathic pain and as adjunctive therapy for focal seizures in patients with epilepsy. In addition, there are a number of conditions for which pregabalin is prescribed off-label. Along with the widespread use there are a significant number of reports describing the misuse of pregabalin over the last decade. Over time, it became clear that pregabalin should become part of routine testing in toxicology laboratories. The aim of this paper was to present validation of a LC-MS/MS method for the quantification of pregabalin in plasma of acutely poisoned patients. Simple sample preparation step and rapid chromatographic separation shortened the overall analysis time, which was the goal of method development. The presence of pregabalin was confirmed with three ion transitions, ensuring high selectivity of the validated method. The statistical data obtained showed good precision and accuracy over a wide concentration range. No endogenous or other interference was detected, and there was no matrix effect influence with this method. The LC-MS/MS method was applied to quantify pregabalin in plasma samples of patients admitted to the emergency department due to a possible acute pregabalin overdose. Different concentrations were found, and we report, to the best of our knowledge, the highest plasma concentration of pregabalin in the plasma of a patient with acute poisoning. In conclusion, we developed a fast and simple LC-MS/MS method for reliable determination of pregabalin and demonstrated the developed method was suitable for routine use in clinical toxicology setting.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41285539","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Polycyclic aromatic hydrocarbons (PAHs) are persistent organic pollutants (POPs) that are widely distributed in the environment and cause significant environmental damage. Furthermore, they endanger human health by polluting food from the natural environment and food processing. Therefore, it is necessary to accurately detect PAHs in various sample matrices, which requires precise, practical, and rapid detection methods. The purpose of this research is to develop a high sensitivity analysis method by analyzing the optimum excitation and emission wavelengths of EPA's 15 priority polyaromatic hydrocarbons in the UHPLC fluorescence detector (Acenaphthene, Anthracene, Benzo[a]anthracene, Benzo[b]fluoranthene, Benzo[k]fluoranthene, Benzo[ghi]perylene, Benzo[a]pyrene, Chrysene, Dibenzo[a,h]anthracene, Fluoranthene, Fluorene, Indeno[1,2,3-cd]pyrene, Naphthalene, Phenanthrene, and Pyrene). An average of 17–25 analyses were performed for each polyaromatic hydrocarbon, and optimized excitation and emission wavelengths were obtained. LOD levels between 2 and 90 ppt were obtained with the method created in this direction. It is worth mentioning that the limits achieved for some PAH parameters are lower than those reported in the literature after pre-concentration steps.
{"title":"Optimization of excitation and emission wavelengths for the UHPLC fluorescence detector for priority polycyclic aromatic hydrocarbons (PAHs)","authors":"B. İzgi, Selman Kander","doi":"10.1556/1326.2023.01118","DOIUrl":"https://doi.org/10.1556/1326.2023.01118","url":null,"abstract":"Polycyclic aromatic hydrocarbons (PAHs) are persistent organic pollutants (POPs) that are widely distributed in the environment and cause significant environmental damage. Furthermore, they endanger human health by polluting food from the natural environment and food processing. Therefore, it is necessary to accurately detect PAHs in various sample matrices, which requires precise, practical, and rapid detection methods. The purpose of this research is to develop a high sensitivity analysis method by analyzing the optimum excitation and emission wavelengths of EPA's 15 priority polyaromatic hydrocarbons in the UHPLC fluorescence detector (Acenaphthene, Anthracene, Benzo[a]anthracene, Benzo[b]fluoranthene, Benzo[k]fluoranthene, Benzo[ghi]perylene, Benzo[a]pyrene, Chrysene, Dibenzo[a,h]anthracene, Fluoranthene, Fluorene, Indeno[1,2,3-cd]pyrene, Naphthalene, Phenanthrene, and Pyrene). An average of 17–25 analyses were performed for each polyaromatic hydrocarbon, and optimized excitation and emission wavelengths were obtained. LOD levels between 2 and 90 ppt were obtained with the method created in this direction. It is worth mentioning that the limits achieved for some PAH parameters are lower than those reported in the literature after pre-concentration steps.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-02-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43451558","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The two chemical components Escitalopram (ESC) and Etizolam (ETZ) are beneficial for the health of individuals because it helps to treat anxiety. The study mainly illustrated that a green approach is essential in the medical sector with the help of “Green Analytical quality by design”. According to AQbD, the techniques of HPTLC have become eco-friendly, and decided to use “ESC” and “ETZ”. Hence, ethanol and phosphate buffer pH 3.5 adjusted with 1% “orthophosphoric acid”. After the retardation factor, the product ESC was found at 0.34 min and ETZ was found at 0.53 min. The linearity of ETZ the range varies from 300 to 1800 μg mL−1 and for ESC it varies from 100 to 600 μg mL−1. The validation parameter of R2 Values ranged from 0.9997 to 0.9994 for both ESC and ETZ. The study also demonstrated that different other methods were also useful for the medical sector to make it more convenient and eco-friendly. Some of those approaches are “GAPI”, “AGMS”, “NEMI”, and “AGREE”. The outcome of the study helped to find that the technique “HPTLC” is a green analytic design that helps to maintain the stability of the medicine and it was also approved as a quality design and also a novel approach in the pharmaceutical sector.
{"title":"Eco-friendly based stability-indicating HPTLC technique for the determination of Escitalopram and Etizolam by employing quality by design approach","authors":"D. Perumal, M. Krishnan, K. Lakshmi","doi":"10.1556/1326.2023.01117","DOIUrl":"https://doi.org/10.1556/1326.2023.01117","url":null,"abstract":"The two chemical components Escitalopram (ESC) and Etizolam (ETZ) are beneficial for the health of individuals because it helps to treat anxiety. The study mainly illustrated that a green approach is essential in the medical sector with the help of “Green Analytical quality by design”. According to AQbD, the techniques of HPTLC have become eco-friendly, and decided to use “ESC” and “ETZ”. Hence, ethanol and phosphate buffer pH 3.5 adjusted with 1% “orthophosphoric acid”. After the retardation factor, the product ESC was found at 0.34 min and ETZ was found at 0.53 min. The linearity of ETZ the range varies from 300 to 1800 μg mL−1 and for ESC it varies from 100 to 600 μg mL−1. The validation parameter of R2 Values ranged from 0.9997 to 0.9994 for both ESC and ETZ. The study also demonstrated that different other methods were also useful for the medical sector to make it more convenient and eco-friendly. Some of those approaches are “GAPI”, “AGMS”, “NEMI”, and “AGREE”. The outcome of the study helped to find that the technique “HPTLC” is a green analytic design that helps to maintain the stability of the medicine and it was also approved as a quality design and also a novel approach in the pharmaceutical sector.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-01-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44822579","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Muhammad Faisal Javed, Manzar Zahra, Iqra Javed, Shahbaz Ahmad, T. Jabeen, Muhammad Ahmad
A new precise, selective and reliable reversed phase high performance liquid chromatographic (RP-HPLC) method has been developed and validated for the determination of Methyl paraben sodium (MPS) and Propyl paraben sodium (PPS) (preservatives) in Iron protein succinylate syrup. Optimized conditions were; Methanol: Water (65: 35) as mobile phase, UV/Vis detector at the wavelength of 254 nm and flow rate was set at 1.3 ml min−1. By applying the set of conditions, separation of components was carried out in less than 7 min for both the analytes. The method was validated according to International conference of Harmonization (ICH) guidelines and the analytical characteristic parameters of validation included specificity, limit of detection (LOD), limit of quantification, linearity, accuracy, precision and robustness were evaluated. The calibration curve was found to be linear in the range of 0.045 mg mL−1 to 0.075 mg mL−1 for Methyl paraben sodium and 0.015 mg mL−1 to 0.025 mg mL−1 for propyl paraben sodium with a correlation coefficient r2 > 0.999. Accuracy; reported as percentage recovery was found to be in the range of 98.71%–101.64% for Methyl paraben sodium and 99.85%–101.47% for Propyl paraben sodium at 80%, 100% and 120% concentration for both the analytes. The proposed method was found to be precise and robust when evaluated by variations in wavelength, mobile phase composition, temperature and analyst. The limit of detection (LOD) was found 0.001 mg mL−1 (3 ppm) for Methyl paraben sodium and 0.001 mg mL−1 (1 ppm) for Propyl paraben sodium.
{"title":"Development and validation of RP HPLC method for the estimation of methyl paraben sodium and propyl paraben sodium in iron protein succinylate syrup","authors":"Muhammad Faisal Javed, Manzar Zahra, Iqra Javed, Shahbaz Ahmad, T. Jabeen, Muhammad Ahmad","doi":"10.1556/1326.2022.00990","DOIUrl":"https://doi.org/10.1556/1326.2022.00990","url":null,"abstract":"A new precise, selective and reliable reversed phase high performance liquid chromatographic (RP-HPLC) method has been developed and validated for the determination of Methyl paraben sodium (MPS) and Propyl paraben sodium (PPS) (preservatives) in Iron protein succinylate syrup. Optimized conditions were; Methanol: Water (65: 35) as mobile phase, UV/Vis detector at the wavelength of 254 nm and flow rate was set at 1.3 ml min−1. By applying the set of conditions, separation of components was carried out in less than 7 min for both the analytes. The method was validated according to International conference of Harmonization (ICH) guidelines and the analytical characteristic parameters of validation included specificity, limit of detection (LOD), limit of quantification, linearity, accuracy, precision and robustness were evaluated. The calibration curve was found to be linear in the range of 0.045 mg mL−1 to 0.075 mg mL−1 for Methyl paraben sodium and 0.015 mg mL−1 to 0.025 mg mL−1 for propyl paraben sodium with a correlation coefficient r2 > 0.999. Accuracy; reported as percentage recovery was found to be in the range of 98.71%–101.64% for Methyl paraben sodium and 99.85%–101.47% for Propyl paraben sodium at 80%, 100% and 120% concentration for both the analytes. The proposed method was found to be precise and robust when evaluated by variations in wavelength, mobile phase composition, temperature and analyst. The limit of detection (LOD) was found 0.001 mg mL−1 (3 ppm) for Methyl paraben sodium and 0.001 mg mL−1 (1 ppm) for Propyl paraben sodium.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-01-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44236072","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Dispersive liquid-liquid microextraction (DLLME) and high performance liquid chromatography – UV detection was presented for extraction and determination of nandrolone and testosterone in human urines. Chloroform at microliter volume level and acetonitrile were used as extraction and dispersive solvents, respectively. The main advantages of method are high speed, high enrichment factor, high recovery, good repeatability and extraction solvent volume at µL level. The influence of several variables (e.g. type and volume of disperser and extraction solvents, ionic strength, etc.) on the performance of the sample preparation step was carefully evaluated. Under the optimum conditions, the calibration graphs were linear in the range of 5–500 μg L−1 with detection limit of 2.5 μg L−1 for both of them. The relative standard deviation (R.S.D.s) for five replicate measurements of nandrolone and testosterone were 9.4% and 8.8%, respectively. The relative recoveries of nandrolone and testosterone in urine sample at spiking level of 25.0 μg L−1 are ranged between 86.4% and 98%. DLLME combined with HPLC-UV is a fast, simple and efficient method for the determination of nandrolone and testosterone in human urines.
{"title":"Dispersive liquid-liquid microextraction followed by high-performance liquid chromatography as an efficient and sensitive technique for determination of nandrolone and testosterone in human urine","authors":"M. Rezaee","doi":"10.1556/1326.2021.00972","DOIUrl":"https://doi.org/10.1556/1326.2021.00972","url":null,"abstract":"Dispersive liquid-liquid microextraction (DLLME) and high performance liquid chromatography – UV detection was presented for extraction and determination of nandrolone and testosterone in human urines. Chloroform at microliter volume level and acetonitrile were used as extraction and dispersive solvents, respectively. The main advantages of method are high speed, high enrichment factor, high recovery, good repeatability and extraction solvent volume at µL level. The influence of several variables (e.g. type and volume of disperser and extraction solvents, ionic strength, etc.) on the performance of the sample preparation step was carefully evaluated. Under the optimum conditions, the calibration graphs were linear in the range of 5–500 μg L−1 with detection limit of 2.5 μg L−1 for both of them. The relative standard deviation (R.S.D.s) for five replicate measurements of nandrolone and testosterone were 9.4% and 8.8%, respectively. The relative recoveries of nandrolone and testosterone in urine sample at spiking level of 25.0 μg L−1 are ranged between 86.4% and 98%. DLLME combined with HPLC-UV is a fast, simple and efficient method for the determination of nandrolone and testosterone in human urines.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-01-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43239358","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Jelena Dokmanović, I. Kasagić-Vujanović, Ž. Gagić, K. Nikolić, Marija Čarapić, D. Agbaba
Using the Design of Experiments methodology (Response-Surface Methodology and Derringer's Desirability Function), a simple, fast and robust RP-HPLC method was developed for the analysis of enrofloxacin (EFC), its impurity A (fluoroquinolonic acid, FQ) and impurity B (ciprofloxacin, CPX). Gradient elution of samples was performed on a Zorbax Eclipse XDB C18 column (150 × 4.6 mm, 3.5 μm) with a mobile phase consisting of 32 mM phosphate buffer pH 3.5 – methanol (0 min-19.6% methanol; 15.5 min-19.6% methanol; 29.5 min-80% methanol; 30 min-19.6% methanol; 35 min-19.6% methanol), delivered at a flow rate of 1.5 mL min−1, wavelength of detection 278 nm (for EFX and CFX) and 265 nm for FQ. A good linear response was achieved in the range 15–35 μg mL−1 (EFX) and LOQ-150% for impurities (CFX and FQ). Other validation parameters were also tested: precision, accuracy, sensitivity and robustness. The developed method was shown to be simple, practical and suitable for the analysis of EFC and its impurities (CPX, FQ) in veterinary drugs.
{"title":"Design of experiments and Derringer's desirability function in optimisation and validation of RP-HPLC method for the analysis of enrofloxacin and its impurities","authors":"Jelena Dokmanović, I. Kasagić-Vujanović, Ž. Gagić, K. Nikolić, Marija Čarapić, D. Agbaba","doi":"10.1556/1326.2022.01111","DOIUrl":"https://doi.org/10.1556/1326.2022.01111","url":null,"abstract":"Using the Design of Experiments methodology (Response-Surface Methodology and Derringer's Desirability Function), a simple, fast and robust RP-HPLC method was developed for the analysis of enrofloxacin (EFC), its impurity A (fluoroquinolonic acid, FQ) and impurity B (ciprofloxacin, CPX). Gradient elution of samples was performed on a Zorbax Eclipse XDB C18 column (150 × 4.6 mm, 3.5 μm) with a mobile phase consisting of 32 mM phosphate buffer pH 3.5 – methanol (0 min-19.6% methanol; 15.5 min-19.6% methanol; 29.5 min-80% methanol; 30 min-19.6% methanol; 35 min-19.6% methanol), delivered at a flow rate of 1.5 mL min−1, wavelength of detection 278 nm (for EFX and CFX) and 265 nm for FQ. A good linear response was achieved in the range 15–35 μg mL−1 (EFX) and LOQ-150% for impurities (CFX and FQ). Other validation parameters were also tested: precision, accuracy, sensitivity and robustness. The developed method was shown to be simple, practical and suitable for the analysis of EFC and its impurities (CPX, FQ) in veterinary drugs.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-01-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49426498","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
M. Ajay Babu, J.V. Shanmukh Kumar, N. Naresh, Sharad D. Mankumare
A rapid, stability indicating reverse phase liquid chromatographic method was developed for the determination of purity of Felodipine in active pharmaceutical substance form in the presence of its impurity and its degradation products. To develop the method which is also compatible to liquid chromatographic mass spectroscopic technique. The developed method is also used to determine the assay of Felodipine in bulk drug form. The drug is subjected to various stress conditions like acidic, basic, oxidation, UV light and thermal conditions. Considerable degradation was observed during base hydrolysis. Two degradation products were identified. The Waters Acquity UPLC BEH C18, 2.1 × 100 mm, 1.7 µm Column was used to achieve chromatographic separation. The gradient conditions, diluent and injection volume were optimized to achieve the acceptable resolution between impurities and its degradation products from Felodipine and to get good peak shapes. The masses were determined for main compound and its identified degradation products. Further, the characterization studies for main compound and its degradation products were performed using LCMSMS Q-TOF.
{"title":"Sensitive and validated UPLC-MS/MS method for the identification and characterization of forced degradation products for felodipine","authors":"M. Ajay Babu, J.V. Shanmukh Kumar, N. Naresh, Sharad D. Mankumare","doi":"10.1556/1326.2022.01106","DOIUrl":"https://doi.org/10.1556/1326.2022.01106","url":null,"abstract":"A rapid, stability indicating reverse phase liquid chromatographic method was developed for the determination of purity of Felodipine in active pharmaceutical substance form in the presence of its impurity and its degradation products. To develop the method which is also compatible to liquid chromatographic mass spectroscopic technique. The developed method is also used to determine the assay of Felodipine in bulk drug form. The drug is subjected to various stress conditions like acidic, basic, oxidation, UV light and thermal conditions. Considerable degradation was observed during base hydrolysis. Two degradation products were identified. The Waters Acquity UPLC BEH C18, 2.1 × 100 mm, 1.7 µm Column was used to achieve chromatographic separation. The gradient conditions, diluent and injection volume were optimized to achieve the acceptable resolution between impurities and its degradation products from Felodipine and to get good peak shapes. The masses were determined for main compound and its identified degradation products. Further, the characterization studies for main compound and its degradation products were performed using LCMSMS Q-TOF.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":null,"pages":null},"PeriodicalIF":1.9,"publicationDate":"2023-01-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43262987","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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