جستجوی مقالات مرتبط با کلیدواژه "capillary electrophoresis" در نشریات گروه "پزشکی"
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Background and Objectives
The possible adverse effect of histamine on human health has made it a detrimental aspect to the quality and safety of many fermented food products especially fish sauce.
Materials and MethodsIn the present study, hdcA gene in Staphylococcus epidermidis TYH1 was knocked out and its effect on histamine production was evaluated. HdcA encodes histidine decarboxylase, an enzyme that produces histamine from histidine. Both strains of TYH1, the wild type (WT) and mutant (∆hdcA) were then incubated in tryptic soy broth (TSB) supplemented with histidine (0.5 mM). The histamine content determined by capillary zone electrophoretic (CZE) analysis. Safety assessment of this mutant of food origin was conferred by virulence genes.
ResultsIt was found that S. epidermidis TYH1 exhibited production of histamine (50.09 ± 0.06 μg/mL), while ∆hdcA strain of TYH1 exhibited no histamine forming activity. Safety assessment of ∆hdcA revealed the presence of nuc gene, while superantigenic toxins and coa genes were not observed. Therefore, it has the ability to be used as a starter culture to decrease the histamine content in any fermented food products.
ConclusionOur study findings may contribute to provide a novel approach of promoting the food safety of fish sauce and other fermented food products regarding the regulation of histamine content.
Keywords: Staphylococcus epidermidis, Histamine, Histidine decarboxylase, Capillary electrophoresis, Enterotoxin -
Objective
Determination of HbA1c level is a precious indicator for therapeutic follow-up of patients with type 1 or type 2 diabetes. Our study aimed to evaluate the analytical characteristics of Capillarys 3 Octa® HbA1c measurement by capillary electrophoresis.
Materials and MethodsOur study involved 265 venous whole blood specimens repeatability, intermediate fidelity, accuracy, linearity, and correlation with the Arkray HA-8180 analyzer which uses HPLC as a dosing method. We studied interferences such as hematocrit, triglycerides, total bilirubin, labile fraction, and hemoglobin abnormalities.
ResultsThe linearity correlation was between 4.4% and 20.3%. There was a strong correlation with HPLC (r > 0.99, P< 0.0001). No interference from hematocrit (20-93%) (P: 0.888), triglycerides (until 25 mmol/L) (P: 0.388), total bilirubin (< 587 µmol/L) (P: 0.993), and labile fraction was observed. No problem related to inter-sample contamination was observed. The sensitivity was zero for homozygous sickle cell disease and S/C composite hemoglobinosis. However, sensitivity was high for heterozygous forms (69% for A/S and 60% for A/C). The analyzer was able to separate and quantify HbA2 fraction, allowing ß-thalassemia accidental detection.
ConclusionCapillarys 3 Octa® based on capillary electrophoresis proved to be precise and a linear instrument for HbA1c measurement. Several clinical interferences and Hb variants had no effect on the results. The results of this evaluation suggest that this analyzer is suitable for routine use in clinical chemistry laboratories.
Keywords: HbA1c, Capillarys 3 Octa®, Capillary electrophoresis, Analytical performance, Hemoglobinopathies -
Biolmpacts, Volume:11 Issue: 4, Jul 2021, PP 263 -369Introduction
A new microfluidic-based method with electrochemical detection was developed for the simultaneous quantification of acetaminophen (AP) and phenylephrine (PHE) pharmaceuticals in the human blood and pharmaceuticals (e.g. tablet and drop).
MethodsThe separation was achieved on a SU8/glass microchip with a 100 µm Pt working electrode that was positioned out of the channel and 2-(N-morpholino) ethanesulfonic acid was used as a running buffer (pH 7, 10 mM). Home designed modulated high voltage power supply and dual time switcher was used for controlling the injection and separation of the analytes in the unpinched injection mode.
ResultsThe injection was carried out using +750 V for 7 seconds, and the separation and detection voltages were set at +1000 V and +0.9 V, respectively. Critical parameters such as detection potential, buffer concentration, injection, and separation voltage were studied in terms of their effects on the resolution, peak height, and migration times. For each analyte, the correlation coefficients were over 0.99 (n=6). The developed microchip was able to detect AP and phenylephrine simultaneously with the limit of detection of 7.9 and 5.2 (µg/mL) respectively for PHE and AP and excellent linear range of 10-200 (µg/mL). The recovery of the drugs ranged from 96% to 103%, while the repeatability of the method through inter- and intra-day was lower than 7%.
ConclusionThe developed method offers several advantages, including easy sample pretreatment process, simplicity, very fast analysis compared to other typical chromatographic methods. Thus, the proposed microfluidic-based method is proposed to be used as a time- and cost-effective monitoring method for the analysis of AP and PHE.
Keywords: Acetaminophen, Electrochemical detection, Microfluidics, Microchip, Capillary electrophoresis, Phenylephrine -
Cardiovascular diseases (CVDs) are the leading cause of mortality worldwide and are usually multifactorial medical conditions. Usually cardiovascular patients must follow a complicated treatment scheme, containing several drugs. Fixed dose combinations (FDCs) are pharmaceutical formulations containing two or more active ingredients in a one pill. FDCs can add multiple benefits to the treatment of CVDs including increased patient compliance, elimination of some side effects and the simultaneous blockage of multiple pathogenic links. The great prevelance of FDCs in modern therapy brings the necessity of developing new analytical methods for the simultaneous analysis of their components. Capillary electrophoresis (CE) was shown to be as a complementary and attractive alternative to the more frequently used chromatographic methods. CE advantages relate to the high efficiency of separation, rapid method developement, short analysis time and relatively low operational costs. The most frequently used CE techniques in the analysis of FDCs are capilllary zone electrophoresis (CZE) for ionized analytes and micellar electrokinetic chromatography (MEKC) for neutral ones. The current article reviews application of CE in the analysis of FDCs used in the treatment of CVDs.
Keywords: fixed dose combination, capillary electrophoresis, Cardiovascular diseases -
There are more than 400 different variations on α-globin protein, and most of them are not associated with noticeable clinical manifestation. Hemoglobin (Hb) is an oxygen-transporting protein and Hb Daneshgah- Tehran is an α-globin variant that for the first time was reported from Iran in a case with normal haematological indices. The capillary electrophoresis of an 8-year- old-girl with normal hematological parameters showed a peak in the location of Hb S (19.2%) with small amount of Hb A2 variant. The sequencing analysis indicated that the patient was heterozygote for Hb Daneshgah- Tehran (HBA1:c.218A>G p.His72Arg). Alpha and beta thalassemia are common health problems in north of Iran, and about 15% of Mazandarani people are carriers for alpha globin gene deletions, hence premarital screening program can help diagnosis of common and rare hemoglobinopathies. This case was the first report on Hb Daneshgah- Tehran from Mazandaran and the second one from Iran. The presented case showed that Hb Daneshgah- Tehran had haematological indices in normal range, and for the detection of this Hb variant, electrophoresis and PCR sequencing methods should be applied.
Keywords: Alpha-globin, Capillary electrophoresis, Hemoglobin -
Tramadol is a widely used opioid analgesic frequently prescribed for treatment of moderate to severe, acute and chronic pain. It has a complex mechanism of action, acting both as a central opiate agonist and as a norepinephrine and serotonin reuptake inhibitor. It is a chiral substance, having two chiral centers in its structure and it is used in therapy as a racemic mixture of two of its enantiomers, (S,S)-tramadol and (R,R)-tramadol. In the last 25 years, several analytical procedures have been published in the literature for the achiral and chiral determination of tramadol from pharmaceutical formulations and biological matrices. Among these methods, capillary electrophoresis techniques have proved to be an efficient, reliable and cost-effective solution. The purpose of the present review is to provide a systematic survey to present and discuss the electrodriven methods available in the literature for the achiral and chiral analysis of tramadol.
Keywords: Tramadol, Capillary electrophoresis, Chiral separation, Pharmaceutical analysis -
BackgroundA micellar electrokinetic chromatographic (MEKC)/ indirect UV detection method with hydrodynamic and electrokinetic injection has been developed for the determination of pregabalin in the serum samples.MethodsSeparation of the drug was achieved on Agilent capillary electrophorese in less than 5 min using a 50 cm × 75 μm i.d. uncoated fused-silica capillary and a background electrolyte (BGE) consisting of 5-aminosalicylic acid (5-ASA, 10 mmol L-1), cetyl trimethylammonium bromide (CTAB, 1 mmol L-1) and tri-sodium citrate (4% w/v). The influence of various parameters on the separation such as separation voltage, injection time, cassette temperature, pH of BGE and organic modifier was investigated.ResultsMethod validation shown good linearity (R2> 0.999) in the range of 1.5-100 µg mL-1 of pregabalin. A limit of detection (LOD) of 0.8 μg mL-1 and a limit of quantitation (LOQ) of 2.6 μg mL-1 were reported for pregabalin.ConclusionThe proposed method was found to be suitable and accurate for the determination of pregabalin in serum samples.Keywords: Field-amplified sample injection, Micellar electrokinetic chromatography, Capillary electrophoresis, Pregabalin
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Background
Non syndromic oculocutaneous albinism type (OCA) is caused by mutations in tyrosinase (TYR), OCA2, TYRP1, MATP (SLC45A2), SLC24A5 and C10ORF11 genes. Screening for mutations is important in families with oculocutaneous albinism patients in order to accurately diagnose the albinism type, genetic counseling and future therapeutic purposes.
ObjectivesThe Aim of this study was to investigate the founder effect of most frequent mutations in OCA patients.
MethodsTYR gene was sequenced in 26 unrelated inbred OCA families as well as 56 unrelated healthy individuals. In addition, homozygosity mapping was performed using 13 STR markers for 6 OCA loci (TYR, OCA2, TYRP1, MATP (SLC45A2), SLC24A5 and C10ORF11 genes). Different mutations were found in these genes from which a single base duplication (c.286dupA) and two single base substitutions c.996G > A (p.M332I) and c.230G > A (p.R77Q) had the most frequencies among the OCA families. In order to investigate the founder effect of these mutations, the haplotypes of two STR markers (TYR-S1 and TYR-S2) inside the TYR gene were ascertained.
ResultsIt was revealed that families with similar mutation harbored similar haplotype for the TYR STR markers too.
ConclusionsWe conclude that these mutations are possible founder mutations in the Iranian population.
Keywords: OCA, TYR, Capillary Electrophoresis, Founder Effect -
A common approach in resolving enantiomers of chiral basic drugs by capillary electrophoresis (CE) is to use cyclodextrins (especially their anionic derivatives) as chiral selector in the acidic buffer (pH ≤ 3) in normal or reversed (carrier) mode. Then, some organic modifiers are added to the buffer solution if the resolution is not satisfactory. In case of cetirizine (CTN), applying the same approach, i.e. a reversed mode capillary zone electrophoresis (CZE) method with an acidic buffer and sulfated-b-cyclodextrine (S-bCD) as chiral selector, was failed and no complete enantioseparation was achieved. Different organic modifiers, like urea and triethylamine HCl, were used to improve chiral resolution which led to partial resolution of the two peaks. Then, guanidine HCl at a concnetration of 100 mM was added to the running buffer and an acceptable resolution of the enantiomers of the drug was obtained. The method was successfully applied to determine optical purity of a levo-cetirizine (l-CTN) sample.Keywords: Cetirizine, Chiral separation, Capillary electrophoresis, Guanidine HCl, Sulfated ?, Cyclodextrin
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BackgroundHemoglobinopathies are the commonest single gene disorder in human that affect hemoglobin production and function that occur when mutations alter the amino acid sequence of globin chains. The purpose of the present study was to evaluate the prevalence of hemoglobninopathies detected by capillary electrophoresis method in individuals referred to Masjed-Soleiman health centers by capillary electrophoresis method.MethodsThis study was carried out on 394 individuals referred to Masjed-Soleiman health centers during 2015-2016. Blood samples were collected in EDTA vacutainer tubes, then CBC including blood indexes (MCV, MCH), level of Hemoglobin A, Hb F, Hb A2 and other hemoglobins were evaluated by Sebia minicap (France) and also genetic tests applied for them to confirm results that were aqcuired by capillary electrophoresis method.Results77 (19.5%) subjects had HbA2 ≥3.5%, thus were classified as beta thalassemia carrier and 3.3%, 2.5%, 1.5% and 0.5% of the individuals were heterozygote for Hb S, Hb D, Hb C and Hb Bart, respectively. Results of the genetic analysis showed the mutations in these subjects; cd36-37(-T) was the most frequent mutation in beta thalassemia carriers in this geographic region.ConclusionThis study showed high frequency of beta thalassemia mutations in the geographic region of Masjed-Soleiman (19.5), and 7.85% of the individuals had hemoglobin variants including Hb S, Hb D and Hb C detected by capillary electrophoresis. Capillary electrophoresis could be a considerable method for detection of hemoglobinopathies.Keywords: Hemoglobinopathy, Capillary electrophoresis, Hemoglobin variants, Beta thalassemia mutations
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The Capillary Electrophoresis (CE) is a very useful technique to determine and to quantify pharmaceutical materials. In this work, a capillary electrophoresis method has been developed for the determination of Cefquinome sulfate in aqueous solution and in biological media (urine, milk and plasma). The ion mobility was measured at the various pH values. The detection limit and the relative standard deviation of migration times of the peak area were determined. The influence of the pH on the separation of Cefquinome sulfate in plasma and in urine was investigated. The SDS micellar elecrokinetic chromatography (SDS-MEKC) was used for the determination of Cefquinome sulfate in water, plasma and urine. The solubility and stability of Cefquinome sulfate were considered at the different pH values. The best stability was found at pH 7.4. Also the hydrophilic/lipophilic properties of Cefquinome sulfate (partition coefficient and permeation, in vitro) were investigated. The hydrophilic properties of cefquinome affected the results; the partition coefficient was 0.01 at pH 7.4. In addition, the permeation coefficient was 1.65 at pH 7.4. Acid the dissociation constant of cefquinome was calculated using CZE. The low amount of sample required and the relatively short analyze time were the main advantages of this method.Keywords: Capillary Electrophoresis, Cefquinome Sulfate, Cephalosporins
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ObjectiveThe phenylalanine hydroxylase (PAH) locus has high linkage disequilibrium. Haplotypes related to this locus may thus be considered sufficiently informative for genetic diagnosis and carrier screening using multi-allelic markers. In this study, we present an efficient method for haplotype analysis of PAH locus using multiplexing dyes. In addition, we explain how to resolve the dye shift challenge in multiplex short tandem repeat (STR) genotyping.Materials And MethodsOne hundred family trios were included in this descriptive study. The forward primer of a tetra-nucleotide STR and the reverse primer of a variable number tandem repeat (VNTR) were labeled with three different non-overlapping dyes 5-carboxyfluorescein (FAM), 6-carboxy-N,N,N,N-tetramethylrhodamine (HEX) and 6-carboxy- N,N,N,N-tetramethylrhodamine (TAMRA). The polymerase chain reaction (PCR) products from each family trio were multiplexed for capillary electrophoresis and results were analyzed using Peak Scanner software.ResultsMultiplexing trio products decreased the cost significantly. The TAMRA labeled products had a significant predictable shift (migrated at a slower electrophoretic rate) relative to the HEX and FAM labeled products. Through our methodology we achieve, the less inter-dye shift than intra-dye shift variance. Correcting the dye shift in the labeled products, according to the reference allele size, significantly decreased the inter-dye variability (PConclusionMultiplexing trio products helps to detect and resolve the dye shift accurately in each family, which otherwise would result in diagnostic error. The dye system of FAM, HEX and TAMRA is more feasible and cheaper than other dye systems.Keywords: Microsatellite Repeats, Fluorescent Dyes, Capillary Electrophoresis, Diagnostic Error, Phenylalanine Hydroxylase
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مجله دانشکده پزشکی دانشگاه علوم پزشکی تهران، سال هفتاد و چهارم شماره 3 (پیاپی 183، خرداد 1395)، صص 147 -158اختلالات هموگلوبینی یکی از شایع ترین اختلالات ارثی در جهان هستند که حدود 7% از جمعیت دنیا و %5-6 از جمعیت ایران، حامل ژن های آن ها هستند. به صورت اتوزومال مغلوب به ارث می رسند و در مناطق مدیترانه ای و بخش بزرگی از آسیا و آفریقا بسیار شایع می باشند. به منظور کنترل اختلالات ارثی هموگلوبینی و پیشگیری از انتقال آن ها به فرزندان می توان از مشاوره ژنتیکی و غربالگری جمعیتی با روش های پیشرفته تر و دقیق تر استفاده نمود. هدف از این مطالعه بیان ویژگی های انواع اختلالات هموگلوبینی شایع در ایران، بیان روش های قابل دسترسی جهت غربالگری آن ها و معرفی بهتر روش کاپیلاری الکتروفورز به عنوان روشی سریع و دقیق، می باشد. اختلالات هموگلوبینی شامل دو گروه تالاسمی ها و واریانت های هموگلوبینی هستند که در اثر اختلال در تولید یا ساختار زنجیره های مختلف گلوبین ایجاد می شوند. هیچ یک از روش های آزمایشگاهی به تنهایی نمی تواند به عنوان یک روش قطعی جهت غربالگری معرفی شوند. برای شناسایی بهتر بایستی داده های کافی فراهم شده و از روش های مختلف مانند ژل الکتروفورز، کروماتوگرافی، ایزوالکتریک فوکوسینگ، کاپیلاری الکتروفورز، یا روش های مولکولی به صورت مکمل استفاده شود. روش کاپیلاری الکتروفورز یک روش دقیق و سریع برای غربالگری می باشد و از طرفی به دلیل عدم توانایی در تفکیک تمامی اختلالات هموگلوبینی، بایستی جهت تایید از روش های بیوشیمیایی، بیوفیزیکی یا مولکولی استفاده شود. بهره گرفتن از روش های غربالگری کاپیلاری الکتروفورز و کروماتوگرافی مایع با کارآیی بالا به عنوان دو روش مکمل، داشتن اطلاعات کافی از انواع اختلالات هموگلوبینی، شرح حال بیمار و شاخص های هماتولوژیکی در شناسایی و تشخیص اختلالات هموگلوبینی بسیار موثر است.کلید واژگان: هموگلوبینوپاتی ها, الکتروفورز کاپیلاری, تالاسمی, تغییرات ساختاری ژنومی, کروماتوگرافی, الکتروفورز, غربالگریHemoglobinopathies are most common inherited disorders in the world; approximately 7 percent of the worldwide population and 5-6 percent of population of Iran are carriers. The hemoglobin disorders inherit as autosomal recessive and are very common in the Mediterranean area and much of the Asia and Africa. The control of this inherited disorders need to genetic counseling and accurate screening by more advanced and more accurate methods. This study explains features of current Iran hemoglobin disorders, nominates the accessible methods for screening them and introduces the capillary zone electrophoresis as a rapid and more accurate method. The required data were extracted of various articles and then for good explanation, current Iran hemoglobinopathies properties were showed in the tables and electropherograms of important hemoglobin disorders in Iran population were provided for help to interpretation results of blood tests by capillary zone electrophoresis method. Hemoglobin disorders are including thalassemias and hemoglobin variants; Disruption in the production and malfunction of globin chains cause types of hemoglobin disorders. We cannot introduce one of clinical laboratory tests as critical and basic method for screening and distinguishing types of inherited hemoglobin disorders as alone. For distinguishing the types of them must be prepared enough information and data of the hemoglobin disorders and for more accurate analysis must be used simultaneously different methods as gel electrophoresis, high performance liquid chromatography, isoelectric focusing, capillary zone electrophoresis or molecular tests. The capillary electrophoresis is an accurate and rapid method for screening types of the hemoglobin disorders. Other side this method cannot analyze all of them, so must be used biochemical, biophysical and molecular methods for confirmation the results. This review showed we can use the capillary electrophoresis and HPLC as two complementary methods for hemoglobinopathies screening. We can analyze by the methods more hemoglobin disorders and decrease more laboratory errors. Moreover, we must have patient history, hematological indices, information and data of types of hemoglobinopathies. The patient history and complete blood count results as red blood cell count, mean corpuscular volume, mean corpuscular hemoglobin and mean corpuscular hemoglobin concentration can be useful and helpful in screening the hemoglobin disorders and then distinguishing all of hemoglobin disorders.Keywords: capillary electrophoresis, chromatography, electrophoresis, genomic structural variation, hemoglobinopathies, screening, thalassemia
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Background And ObjectiveNormal hemoglobin (Hb) is formed of a heme group and a protein group known as globin. Globin is made of four polypeptide chains and in hemoglobinopathies, the structure of one of these four polypeptide chain becomes abnormal. Cellulose acetate method is a common way to differentiate haemoglobinopathies. Inability to identify the components of Hb low concentrations and incapability to isolate all Hb types are among the disadvantages of this method. The aim of this study was to report the prevalence of hemoglobinopathies in the North of Iran by capillary electrophoresis method.MethodsAll patients with suspected hemoglobinopathies, referred by physicians for electrophoresis, have been studied in a private center in the city of Gorgan, Iran. The level of HbA2, HbA, HbF and other Hb was recorded.ResultsOverall, 725 blood samples were analyzed using the capillary method. HbE was reported in 2 patients, HbH was observed in 2 patients and Hb Barts was reported in 3 patients. Using the capillary method, among patients with the SDG area, only 4 of 38 (10.52%) had HbS and the majority of them (89.48%) had HbD.ConclusionHbD is the most common hemoglobinopathy in the North of Iran.Keywords: Hemoglobinopathy, hemoglobin D, Capillary Electrophoresis, Iran
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Currently, there is a remarkable interest in the separation and quantification of enantiomeric compounds because of their importance in biochemistry, therapeutic drug monitoring (TDM), pharmaceutical, forensic, etc. In past decades the pharmacopoeia was governed by racemates, but nowadays the U.S. Food and Drug Administration (FDA) exclusively has been issued a statement that racemic new drugs could not be marketed unless they are thoroughly investigated of the pharmacologic and toxicological properties of pure enantiomers. Demands for accurate and precise analytical method for separation and determination of drugs enantiomers and their metabolites in biological fluids are highlighted. Capillary zone electrophoresis (CZE) is an interesting technique that shows promise for the resolution of enantiomers. This is carried out by adding suitable chiral selector to the background electrolyte results to enantioseparation. According to WHO organization report, cardiovascular diseases (CVDs) rank the leading cause of death, globally. Therefore the related risk factors addressing CVDs should be considered and diagnose to prevent the disease. This article provides a brief review on applying off-line and on-line sample preconcentration methods for enhancing the detection limit of cardiovascular drugs.Keywords: Enantiomers, Cardiovascular drugs, Biological fluids, Capillary electrophoresis, Off, line pre, concentration, On, line pre, concentration
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Human interferons (IFNs) are key cytokines secreted by immune system. They have several effects such as antiviral and anti tumors activity, activating immune cells and healing of multiple sclerosis. The type IFNs present in humans are α, β and Υ. IFN β is a polypeptide, normally produced by fibroblasts and seems to be more species-specific than IFN . Structural properties of I FNs are important for their biologic effects. There are a few analytical techniques for separation, identification and determination of IFNs in its formulations such as mass spectroscopy, RP-HPLC and capillary electrophoresis (CE). In this study we used Micellar Electrokinetic Chromatography (MEKC) as a unique mode of CE because of its capability to separate neutral as well as charged solutes. In MEKC, ionic surfactants are added to the running buffer to form micelles which have a three-dimensional structure with the hydrophobic moieties. The selectivity of MEKC can be controlled by the choice of surfactant and also by the addition of modifiers to the buffer. We used sodium tetraborate (Borax) as buffer without any modifier and sodium dodecyl sulfate (SDS) as surfactant. The validated method was used for determination of the IFN β-1b formulation which are manufactured in Iran. From 9 collected different batches, all of them had acceptable potency as claimed on their label with average 102.25 ± 10.030 %. This is the first time that a MEKC method is introduced for quantification of IFN β-1b in its pharmaceutical dosage forms. The method is reliable safe, rapid and accurate.Keywords: Analysis, Capillary Electrophoresis, MEKC, Interferon, ZIFERON®
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PurposeAmlodipine is a long acting, dihydropyridine type calcium channel blocker frequently used in the treatment of hypertension and coronary insufficiency. The calcium channel blocking activity resides primarily in the S-amlodipine enantiomer, while R-amlodipine is a potent inhibitor of smooth muscle cell migration.MethodsIn this study capillary electrophoresis was applied for the enantiomeric separation of amlodipine using different native and derivatized; neutral and charged cyclodextrines as chiral selectors. The effects of pH and composition of the background electrolyte, concentration and type of chiral selector, capillary temperature, running voltage and injection parameters have been investigated.ResultsStereoselective interactions were observed when using α-CD, β-CD, HP-β-CD, RAMEB, CM-β-CD and SBE-β-CD. Optimized separation conditions consisted on a 50 mM phosphate buffer, pH – 3.0, 20 mM RAMEB as chiral selector, + 25 kV applied voltage, 15°C temperature and UV detection at 238 nm. Using the optimized electrophoretic conditions we succeeded the chiral separation of amlodipine enantiomers in approximately 6 minute, the order of migration being R-amlodipine followed by S-amlodipine. The method was successfully applied for the determination of amlodipine enantiomers from commercially available pharmaceuticals. The linearity range, limits of detection and quantification, precision and accuracy were determined and the results obtained confirmed that the method was suitable for this purpose.ConclusionIt can be concluded that the proposed capillary electrophoresis methods can be useful for routine pharmaceutical applications with benefits of its effectivity, simplicity, short analysis time and low consumption of analytes, solvents and chiral selectors.Keywords: Amlodipine, Capillary electrophoresis, Chiral Separation, Cyclodextrines
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Carvedilol is administered as a racemic mixture of the R(+)- and S(-)-enantiomers, although it was demonstrated that the two enantiomers exhibit different pharmacological effects and stereoselective pharmacokinetics. The aim of this study was the evaluation of several native and derivatized cyclodextrines as chiral selectors for the separation of carvedilol enantiomers. Stereoselective interactions were observed with four cyclodextrines (β-CD, hydroxypropyl-β-CD, randomly methylated β-CD and sulfobuthyl ether- β-CD). The effects of CD concentration, pH value and composition of the background electrolyte, capillary temperature, running voltage and injection parameters have been investigated. The method was validated for precision of peak-area response, linearity range and limits of detection and quantification. An efficient stereoselective capillary zone electrophoretic method was developed for the determination of carvedilol enantiomers using a simple 25 mM phosphate buffer at a pH = 2.5 and 10 mM β-CD as chiral selector, resulting in baseline separation of the two enantiomers with sharp peaks and relatively short analysis time. Highly satisfactory results were obtained from the analysis of carvedilol from tablets, indicating that the method is suitable for routine analysis of carvedilol in pharmaceutical products.Keywords: carvedilol, Capillary Electrophoresis, chirality, cyclodextrines, enantiomer separation
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A capillary electrophoresis method was used for assay of some degradation products of carvedilol. The optimized parameters were as; running buffer 80 mM acetate dissolved in methanol/ethanol mixture (65:35 v/v), applied voltage of 19 kV, temperature is 20 ºC and the wavelength range of 200-350 nm. The results indicate that the proposed CE method could effectively separate carvedilol from its degradation products and can be employed as a stability indicating assay method. In addition, the presence of a new unknown degradation product was discovered by this method. In addition, CE behaviour of carvedilol in photo/force degradation conditions gave valuable information concerning the dissimilarities of their ionization. Results indicated that the CE proposed method can be used for the determination of carvedilol in human serum. Finally, accuracy of the proposed method was established by recovery experiments from spiked human serum samples.Keywords: capillary electrophoresis, carvedilol, binary solvent, degradation
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PurposeIndapamide is probably the most frequently prescribed diuretic drug, generally being used for the treatment of hypertension. It contains a chiral center in its molecule; is marketed as a racemic mixture; but there are rather few studies regarding the pharmacokinetic and the pharmacological effect differences of the two enantiomers. Our aim was the development of a simple, rapid and precise analytical procedure for the chiral separation of indapamide enantiomers.MethodsIn this study capillary zone electrophoresis was used for the enantiomeric separation of indapamide using a systematic screening approach involving different native and derivatized; neutral and charged cyclodextrines as chiral selectors. The effects of pH value and composition of the background electrolyte, capillary temperature, running voltage and injection parameters have been investigated.ResultsAfter preliminary analysis a charged derivatized CD, sulfobuthyl ether- β-CD, proved to be the optimum chiral selector for the enantioseparation. Using a buffer solution containing 25 mM disodium hydrogenophosphate – 25 mM sodium didydrogenophosphate and 5 mM sulfobuthyl ether- β-CD as chiral selector at a pH - 7, a voltage of + 25 kV, temperature 15°C and UV detection at 242 nm, we succeeded in the separation of the two enantiomers in approximately 6 minutes, with a resolution of 4.30 and a separation factor of 1.08.ConclusionCapillary zone electrophoresis using cyclodextrines as chiral selectors proved to be a suitable method for the enantioseparation of indapamide. Our method is rapid, specific, reliable, and cost-effective and can be proposed for laboratories performing indapamide routine analysis.Keywords: Indapamide, Capillary electrophoresis, Chiral separation, Cyclodextrines
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