Acta Chromatographica最新文献

{"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":" ","pages":""},"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}

{"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":" ","pages":""},"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}

{"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":" ","pages":""},"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}

{"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":" ","pages":""},"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}

{"title":"UPLC-MS/MS analysis of SZJ-1207 in mouse plasma and brain and application in pharmacokinetic studies","authors":"D. Qi, Yingying Sun, Bingying Hu, Hai An, Haiyang Lin, Jinjun Fang, Yang Wei","doi":"10.1556/1326.2022.01102","DOIUrl":"https://doi.org/10.1556/1326.2022.01102","url":null,"abstract":"SZJ-1207 is an antidepressant natural product with a steroidal structure extracted from Stephanotis mucronata. It is a novel antidepressant candidate molecule and all its pharmacokinetic properties have not been reported. In this pharmacokinetic study in mice following oral administration, an accurate and sensitive UPLC-MS/MS method was established and evaluated to measure SZJ-1207 concentrations in mouse plasma and brain samples. The results provide information regarding the pharmacokinetics of SZJ-1207 as a potential antidepressant.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2023-01-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45255314","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}

{"title":"Analysis of scopolamine and its related substances by means of high-performance liquid chromatography","authors":"D. Obradović, Ivana Pešić, Marija Čarapić, S. Lazović, D. Agbaba","doi":"10.1556/1326.2022.01107","DOIUrl":"https://doi.org/10.1556/1326.2022.01107","url":null,"abstract":"The retention behaviour of scopolamine (hyoscine) and its related compounds (norhyoscine, atropine, homatropine, and noratropine) was investigated on the silica-based HPLC stationary phase. The retention of investigated tropane alkaloids was interpreted by using the Soczewiński-Wachtmeister equation. A high correlation between the retention parameter (log k) and lipophilicity (log P) (R = 0.9923) confirms the significant influence of hydrophobic interactions on the retention behaviour of the aforementioned compounds. It was found that by increasing the acetonitrile fraction, a decrease in retention of the more polar epoxide derivatives (scopolamine, norhyoscine) and an increase in retention of the more lipophilic derivatives (atropine, noratropine, homatropine) is obtained. The best separation of the tropane alkaloids was achieved by a simple procedure that involved a mobile phase composed of acetonitrile and 40 mM ammonium acetate/0.05% TEA, pH 6.5; 50:50 v/v. Selected conditions were assumed for the determination of scopolamine hydrochloride in the eye drops (Scopolamini hydrobromidum 0.25%). The method was validated and it was found as selective, sensitive, precise, accurate, and robust for the further qualitative analysis of the scopolamine-related compounds.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-12-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46500174","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}

{"title":"Isolation and characterization of major degradants in dihydroergotamine injection","authors":"Praveen Basappa, U. Ms, V. Dama","doi":"10.1556/1326.2022.01095","DOIUrl":"https://doi.org/10.1556/1326.2022.01095","url":null,"abstract":"In this study, we report the systematic approach for characterization of two major degradant impurities, which are not listed in any compendia and were formed during the stability studies of Dihydroergotamine mesylate injection (DHE). An ion-pair UPLC chromatographic method was developed to quantify the related substances present in the DHE injection drug product. The same was used to monitor the impurity profiling during its stability. The two unknown impurities were observed at RRT about 0.08 (Impurity-1) and RRT about 0.80 (Impurity-5) and found to be significantly increasing on stability. Forced degradation studies revealed the nature of the impurity and conditions required for enriching them. A Mass compatible HPLC method was developed to quantify only these two impurities using 25% ammonia and formic acid in water. Their mass numbers were identified using LC MS/MS with triple quadruple mass spectrometer coupled with a HPLC. These two impurities were then isolated from enriched products using preparative HPLC. These impurities were then characterized using Mass and NMR analysis along with Q-TOF elemental analysis.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-12-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42010689","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}

{"title":"High-performance liquid chromatography evaluation of lipophilicity and QSRR modeling of a series of dual DNA gyrase and topoisomerase IV inhibitors","authors":"V. Dobričić, J. Savić, T. Tomašič, Martina Durcik, Nace Zidar, L. P. Mašič, J. Ilaš, D. Kikelj, O. Čudina","doi":"10.1556/1326.2022.01096","DOIUrl":"https://doi.org/10.1556/1326.2022.01096","url":null,"abstract":"Bacterial DNA gyrase and topoisomerase IV control the topological state of DNA during replication and represent important antibacterial drug targets. To be successful as drug candidates, newly synthesized compounds must possess optimal lipophilicity, which enables efficient delivery to the site of action. In this study, retention behavior of twenty-three previously synthesized dual DNA gyrase and topoisomerase IV inhibitors was tested in RP-HPLC system, consisting of C8 column and acetonitrile/phosphate buffer (pH 5.5 and pH 7.4) mobile phase. logD was calculated at both pH values and the best correlation with logD was obtained for retention parameter φ0, indicating that this RP-HPLC system could be used as an alternative to the shake-flask determination of lipophilicity. Subsequent QSRR analysis revealed that intrinsic lipophilicity (logP) and molecular weight (bcutm13) have a positive, while solubility (bcutp3) has a negative influence on this retention parameter.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-12-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44524197","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}

{"title":"Optimized ultra-high-performance liquid chromatography tandem mass spectrometry method for detecting compositional changes in Eucommia ulmoides and Achyranthes bidentata paired decoctions in vitro and in vivo","authors":"Chun Chen, L. Lv, Yueying Huang, Mingzhu Gao, Xue Jiang, Xiaoying Ge, D. Zheng, L. Bao","doi":"10.1556/1326.2022.01090","DOIUrl":"https://doi.org/10.1556/1326.2022.01090","url":null,"abstract":"The bark of Eucommia ulmoides and the roots of Achyranthes bidentata are commonly used in traditional Chinese medicine, and their pairing appears in many traditional Chinese medicine formulas as a recognized compatible unit. However, the changes and interactions of the main components of these two formulas when paired remain unclear, and there is currently no standard or method for their quality control and assessment of pharmacological effects.An optimized ultra-high-performance liquid chromatography triple-quadrupole mass spectrometry (UHPLC-MS/MS) method was established for the simultaneous identification of 10 components in E. ulmoides and A. bidentata using in vitro and in vivo models. Tributyltin methacrylate was the internal standard solution, and the blood samples were treated by an organic solvent precipitation method. Gradient elution was conducted on a C18 column at 25 °C with 0.1% formic acid water:acetonitrile as the mobile phase at a flow rate of 0.5 mL min−1. Dynamic multiple response monitoring was performed in negative-ion mode using an Agilent Jet Stream electrospray ionization ion source.In negative-ion detection mode, eucommiol exhibited a good response, and the isomers ginsenoside Ro and achyranthoside C could also be well separated. The developed method accurately detected the five components with a low blood content. Compared to controls, the levels of ginsenoside Ro, chikusetsusaponin Ⅳa, and achyranthoside C increased; the contents of geniposidic acid and pinoresinol diglucoside were unchanged; and the levels of eucommiol, geniposide, β-ecdysterone, genipin, and achyranthoside D decreased in vitro. In vivo, the contents of geniposidic acid, geniposide, pinoresinol diglucoside, and β-ecdysterone were reduced; the contents of eucommiol and ginsenoside Ro were unchanged; and those of achyranthoside D, chikusetsusaponin Ⅳa, and achyranthoside C increased compared to the corresponding levels in the internal control.A method for the quality control of the E. ulmoides-A. bidentata drug pair was established for the first time and the main components in 10 drug pairs could be determined simultaneously in vitro and in vivo. These findings show that the E. ulmoides and A. bidentata drug pair cause a compositional change, providing new ideas for the development of this combination to improve clinical efficacy.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-11-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44905685","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}

{"title":"A sensitive, heart-cutting, two-dimensional liquid chromatography–tandem mass spectrometry method for the determination of mometasone furoate in human plasma: Application for a bioequivalence study in nasal spray formulations","authors":"Leting Yang, Hongyi Yang, Hui-ru Xie, Hui Liu, Gangmin He, Wenjing Zhong, Ling Wang","doi":"10.1556/1326.2022.01088","DOIUrl":"https://doi.org/10.1556/1326.2022.01088","url":null,"abstract":"We developed and validated a sensitive, heart-cutting, two-dimensional liquid chromatography–tandem mass spectrometry (2D-LC‒MS/MS) method to determine the concentration of mometasone furoate in human plasma after nasal spray administration. Isotopically labeled mometasone furoate-13C,d6 was used as an internal standard (IS). Plasma samples were prepared using a solid-phase extraction (SPE) method. With this 2D-LC strategy, the analytes were trapped in the first dimension (1D) column, and only judiciously selected portions of the 1D effluent were transferred to the second dimension (2D) column for further separation to obtain high-resolution information. MS/MS quantification was performed in positive ionization mode via multiple-reaction monitoring (MRM). This analytical method was fully validated according to related regulatory guidance, and the results showed that the method is robust and sensitive enough for pharmacokinetic investigation of mometasone furoate with satisfactory linearity from 0.25 to 30 pg mL−1. This method was successfully applied to a bioequivalence (BE) study of mometasone furoate aqueous nasal sprays in healthy volunteers.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-11-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41858685","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}