Simultaneous Estimation of Escitalopram and Clonazepam in Tablet Dosage Forms Using HPLC-DAD Method and Optimization of Chromatographic Conditions by Box-Behnken Design.
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SUBMITTER: Foudah AI
PROVIDER: S-EPMC9268709 | biostudies-literature |
REPOSITORIES: biostudies-literature
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Project description:Box-Behnken Design is a useful tool for the optimization of the chromatographic analysis. The goal of this study was to select the most significant factors that influenced the following parameters of the chromatographic separation: retention time, relative retention time, symmetry of the peaks, tailing factor, a number of theoretical plates, Foley - Dorsey parameter, resolution factor, peak width at half height. The results underwent the ANOVA test to find the statistically significant variables and interactions between them. The level of significance was for p < 0.05. The polynomial equations described quantitatively the statistically significant parameters and the interactions between them. The statistical analysis indicated both the best conditions for the separation of the compounds and the variables that were most influential for peaks' parameters. The four-factor analysis performed for LEVO and MOXI indicated that ACN, TEA and pH are the most significant factors that influence the separation. The analysis for the pair CIPRO and LEVO required six factors. The statistical analysis proved that the most significant factors are ACN, MeOH and TEA. In the separation of these two compounds on the HPLC column, the interaction ACN × MeOH was also significant.
| S-EPMC6923357 | biostudies-literature
Project description:Background:Danmu preparations (Danmu Capsule and Danmu Syrup), which are made from Nauclea officinalis stem extracts, have good clinical efficacy in acute tonsillitis, acute pharyngitis and upper respiratory tract infection. However, there is currently no reliable and systematic method to control the quality of these two Danmu preparations. Methods:Using high-performance liquid chromatography (HPLC) coupled with diode array detection (DAD), the fingerprints of the Danmu preparations were established at 250 nm to comprehensively investigate the stability of preparation process. The chemical constituents in the Danmu preparations were separated and identified by HPLC coupled with quadrupole-time-of-flight high-definition mass spectrometry (HPLC-Q-TOF-MS). And seven major components were simultaneously determined at dual wavelengths (250 nm, 326 nm). Results:The results of HPLC fingerprint similarity evaluation showed that the similarity values of 25 batches of Danmu preparations were more than 0.993. Twenty-three compounds, including 10 alkaloids, 6 phenolic acids, 2 iridoids, and 5 unknown compounds, were identified or tentatively characterized according to the retention times and MS/MS fragment patterns of compounds. The developed assay method of seven components was validated with acceptable linearity, precision, repeatability, stability and recovery. The contents of strictosamide belonging to alkaloids as the most abundant constituent in Danmu Capsule and Danmu Syrup were 43,681.20-99,652.49 ?g/g and 1567.83-2427.25 ?g/mL respectively. The contents of protocatechuic acid which were the highest in measured phenolic acids were 2633.01-7739.78 ?g/g in Danmu Capsule and 192.05-448.71 ?g/mL in Danmu Syrup, respectively. As an iridoid, the contents of sweroside in Danmu Capsule and Danmu Syrup were 1573.82-2789.81 ?g/g and 70.32-182.81 ?g/mL, respectively. Conclusion:The established qualitative analysis method of fingerprint can be used to attain standardization, uniformity and stability of the preparation process. Meanwhile, the quantitative analysis in this study can be used as an accurate assay method for preparations.
| S-EPMC7027017 | biostudies-literature
Project description:IntroductionPirfenidone film-coated tablets were developed to offer an alternative to the marketed capsule formulation. This study assessed the bioequivalence of the tablet and capsule formulations under fed and fasted states.MethodsA Phase I, open-label, randomized, four-treatment-period, four-sequence, crossover pharmacokinetics study (NCT02525484) was conducted. Each subject received an 801-mg single dose of pirfenidone as three 267-mg capsules or one 801-mg tablet under fasted and fed conditions. Pirfenidone plasma C max, AUC0-t and AUC0-? were used to assess bioequivalence.ResultsForty-four subjects were randomized to treatment. The 801-mg tablet in the fasted state met bioequivalence criteria [90% confidence intervals (CI) 80.00-125.00%] for the GLSM ratios of natural log-transformed C max, AUC0-t and AUC0-?. Under fed conditions, the 801-mg tablet met the bioequivalence criteria for AUC0-t and AUC0-?, but slightly exceeded the bioequivalence criteria for the C max (90% CI of 108.26-125.60%). The tablet C max was approximately 17% higher than that of the capsules. In the fed state, the tablet C max, and both AUC0-t and AUC0-? were reduced by 39% and 17%, respectively, relative to the fasted state. The tablet and capsules had acceptable tolerability profiles.ConclusionsThe pirfenidone 801-mg tablet met bioequivalence criteria when compared with three 267-mg capsules in the fasted state. The tablet C max was slightly higher relative to capsules in the fed state, but this is not expected to have a clinically meaningful impact on the benefit-risk profile of pirfenidone.FundingThis work was supported by F. Hoffmann-La Roche Ltd.
| S-EPMC5599448 | biostudies-literature
Project description:Background: Determination of psychotropic drugs in clinical study is significant, and the establishment of methodologies for these drugs in biological matrices is essential for patients' safety. The search for new methods for their detection is one of the most important challenges of modern scientific research. The methods for analyzing of psychotropic drugs and their metabolites in different biological samples should be based on combining a very efficient separation technique including high-performance liquid chromatography (HPLC), with a sensitive detection method and effectively sample preparation methods. Objective: Retention, peaks symmetry and system efficiency of vortioxetine on Hydro RP, Polar RP, HILIC A (with silica stationary phase), HILIC-B (with aminopropyl stationary phase), and ACE HILIC-N (with polyhydroxy stationary phase and SCX columns were investigated. Various mobile phases containing methanol or acetonitrile as organic modifiers and different additives were also applied to obtained optimal retention, peaks shape, and systems efficiency. The best chromatographic procedure was used for simultaneous analysis of vortioxetine and its metabolites in human serum, urine and saliva samples. Methods: Analysis of vortioxetine was performed in various chromatographic systems: Reversed phase (RP) systems on alkylbonded or phenyl stationary phases, hydrophilic interaction liquid chromatography (HILIC), and ion-exchange chromatography (IEC). Based on the dependence of log k vs the concentration of the organic modifier, log kw values for vortioxetine in various chromatographic systems were determined and compared with calculated log P values. Solid phase extraction (SPE) method was applied for sample pre-treatment before HPLC analysis. HPLC-QTOF-MS method was applied for confirmation of presence of vortioxetine and some its metabolites in biological samples collected from psychiatric patient. Conclusions: Differences were observed in retention parameters with a change of the applied chromatographic system. The various properties of stationary phases resulted in differences in vortioxetine retention, systems' efficiency, and peaks' shape. Lipophilicity parameters were also determined using different HPLC conditions. The most optimal systems were chosen for the analysis of vortioxetine in biological samples. Both serum and urine or saliva samples collected from patients treated with vortioxetine can be used for the drug determination. For the first time, vortioxetine was detected in patient's saliva. Obtained results indicate on possibility of application of saliva samples, which collection are non-invasive and painless, for determination and therapeutic drug monitoring in patients.
| S-EPMC7321162 | biostudies-literature
Project description:Kaixin Powder (KXP) is a classic formula for treating morbid forgetfulness in ancient China. To guarantee the efficacy and safety of KXP, a simple and accurate HPLC-DAD method has been established and validated for the quantitative analysis of seven bioactive compounds in KXP. Dehydrotumulosic acid (DTU) and dehydrotrametenolic acid (DTR) were quantified in KXP for the first time. Good chromatographic separation was conducted on a Kromasil 100-5 C18 column (250 mm × 4.6 mm, 5 μm) by gradient elution using mobile phases containing acetonitrile and 0.1% formic acid aqueous solution at different detection wavelengths. The calibration curves of each compound showed good linearity (r ≥ 0.9990), and the LOD and LOQ were in the ranges of 0.01-0.10 and 0.03-0.40 μg/mL, respectively. The relative standard deviations (RSDs) of intra-day and inter-day precisions were in the ranges of 0.45-1.74% and 0.56-2.32%, respectively. All recoveries were in the range of 93.6-105.5% with an RSD no more than 2.77%. These quantification results of seven compounds determined in the samples were further confirmed by HPLC-QTOF-MS/MS. This study provides a useful and simple method for analyzing the major bioactive compounds and improves the quality assessment research of KXP.
| S-EPMC8153899 | biostudies-literature
Project description:Fringed sagewort (Artemisia frigida Willd., Compositae family) is a well-known medicinal plant in Asian medical systems. Fifty-nine hydroxycinnamates and flavonoids have been found in A. frigida herbs of Siberian origin by high-performance liquid chromatography with diode array and electrospray triple quadrupole mass detection (HPLC-DAD-ESI-QQQ-MS). Their structures were determined after mass fragmentation analysis as caffeoylquinic acids, flavone O-/C-glycosides, flavones, and flavonol aglycones. Most of the discovered components were described in A. frigida for the first time. It was shown that flavonoids with different types of substitution have chemotaxonomic significance for species of Artemisia subsection Frigidae (section Absinthium). After HPLC-DAD quantification of 16 major phenolics in 21 Siberian populations of A. frigida and subsequent principal component analysis, we found substantial variation in the selected compounds, suggesting the existence of two geographical groups of A. frigida. The antioxidant activity of A. frigida herbal tea was determined using 2,2-diphenyl-1-picrylhydrazyl free radical (DPPH•) and hydrophilic/lipophilic oxygen radical absorbance capacity (ORAC) assays and DPPH•-HPLC profiling, revealing it to be high. The effect of digestive media on the phenolic profile and antioxidant capacity of A. frigida herbal tea was assessed under simulated gastrointestinal digestion. We found a minor reduction in caffeoylquinic acid content and ORAC values, but remaining levels were satisfactory for antioxidant protection. These results suggest that A. frigida and its food derivate herbal tea could be recommended as new plant antioxidants rich in phenolics.
| S-EPMC6720735 | biostudies-literature
Project description:Glucosinolates are well known as natural antimicrobials and anticarcinogenic agents. However, these compounds can lose their properties and transform into antinutrients, depending on processing conditions. In addition, the bitterness of some glucosinolate in rapeseed meal can affect the likability of the final product. Therefore, it is important to identify and determine each glucosinolate and its derived form, not just the total glucosinolate content, in order to evaluate the potential of the final rapeseed protein product. This study provides a comprehensive report of the types and quantities of glucosinolates and their derived forms (isothiocyanates) associated with different rapeseed processing conditions. Glucosinolates and isothiocyanates were determined by HPLC-DAD-qTOF. In our study, the enzymatic degradation of glucosinolates by myrosinase was the main factor affecting either glucosinolate or isothiocyanate content. Other factors such as pH seemed to influence the concentration and the presence of glucosinolates. In addition, process parameters, such as extraction time and separation technology, seemed to affect the amount and type of isothiocyanates in the final protein extracts. Overall, both determined intact glucosinolates and their derived forms of isothiocyanates can give different types of biological effects. More studies should be performed to evaluate the impact of glucosinolates and isothiocyanates on human health.
| S-EPMC8622084 | biostudies-literature
Project description:Felbinac, an active pharmaceutical ingredient (API) used clinically for the treatment of osteoarthritis, has poor solubility. Felbinac cataplasm product design was investigated using rheological and mechanical analyses. Experiments using a response surface methodology based on Box?Behnken design (BBD) incorporated three independent variables: the proportions of partially neutralized polyacrylate (NP800), dihydroxyaluminum aminoacetate (DAAA), and felbinac. Statistically significant quadratic models obtained using BBD demonstrated optimal NP-800, DAAA, and felbinac cataplasm proportions of 4.78?5.75%, 0.30?0.59%, and 0.70?0.90%, respectively. Felbinac cataplasms exhibited "gel-like" mechanical property with predominantly elastic behavior. Rheological studies correlated increasing NP-800 and DAAA concentrations with increased complex modulus (G*) values that were inversely related to peeling strength. Frequency sweep and creep tests revealed decreasing tan ? values with increasing NP-800 and DAAA concentrations. G' and G" values were higher for higher NP-800 and DAAA levels, although G" values decreased with increasing DAAA concentration. Response surface methodology was applied to develop mathematical models. Variance analysis showed that the quadratic model effectively predicted felbinac and matrix material interactions, with two verification samples upholding model predictions. Relative errors between predicted and measured G* values were 3.28% and 1.10% and for peeling strength were 1.24% and 5.59%, respectively. In conclusion, rheological and mechanical analyses of felbinac cataplasms using BBD permits optimization of cataplasms as topical drug delivery vehicles.
| S-EPMC6161182 | biostudies-literature
Project description:In this study, a CoO-Fe2O3/SiO2/TiO2 (CIST) nanocomposite was synthesized and utilized as an adsorbent to remove methylene blue (MB), malachite green (MG), and copper (Cu) from aqueous environments. The synthesized nanocomposite was characterized using field emission scanning electron microscopy (FE-SEM), Fourier-transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and X-ray diffraction (XRD). Input parameters included pH (3-10), contact time (10-30 min), adsorbent amount (0.01-0.03 g), and pollutant concentration (20-60 mg L-1). The effects of these parameters on the removal process efficiency were modeled and optimized using the response surface methodology (RSM) based on the Box-Behnken design (BBD). The RSM-BBD method demonstrated the capability to develop a second-degree polynomial model with high validity (R2 ˃ 0.99) for the removal process. The optimization results using the RSM-BBD method revealed a removal efficiency of 98.01%, 93.06%, and 88.26% for MB, MG, and Cu, respectively, under optimal conditions. These conditions were a pH of 6, contact time of 10 min, adsorbent amount of 0.025 g, and concentration of 20 mg L-1. The synthesized adsorbent was recovered through five consecutive adsorption-desorption cycles using hydrochloric acid. The results showed an approximately 12% reduction from the first to the seventh cycle. Also, MB, MG, and Cu removal from real water samples in optimal conditions was achieved in the range of 81.69-98.18%. This study demonstrates the potential use of CIST nanocomposite as an accessible and reusable option for removing MB, MG, and Cu pollutants from aquatic environments.
| S-EPMC10960869 | biostudies-literature
Project description:Increases in testosterone use and mixed reports of adverse events have raised concerns about the cardiovascular safety of testosterone. Testosterone is available in several delivery mechanisms with varying pharmacokinetics; injections cause spikes in testosterone levels, and transdermal patches and gels cause more subtle but sustained increases. The comparative cardiovascular safety of gels, injections, and patches has not been studied.To determine the comparative cardiovascular safety of testosterone injections, patches, and gels.A retrospective cohort study was conducted using administrative claims from a commercially insured (January 1, 2000, to December 31, 2012) and Medicare (January 1, 2007, to December 31, 2010) population in the United States and general practitioner records from the United Kingdom (January 1, 2000, to June 30, 2012). Participants included men (aged ?18 years) who initiated use of testosterone patches, gels, or injections following 180 days with no testosterone use. Our analysis was conducted from December 11, 2013, to November 12, 2014.New initiation of a testosterone dosage form, with use monitored for up to 1 year.Inpatient or outpatient medical records, diagnoses, or claims for cardiovascular and cerebrovascular events including myocardial infarction (MI), unstable angina, stroke, and composite acute event (MI, unstable angina, or stroke); venous thromboembolism (VTE); mortality; and all-cause hospitalization.We identified 544,115 testosterone initiators between the 3 data sets: 37.4% injection, 6.9% patch, and 55.8% gel. The majority of men in the Medicare cohort were injection initiators (51.2%), most in the US commercially insured population were gel initiators (56.5%), and the UK database included equal proportions of injections and gel users (approximately 41%). With analysis conducted using hazard ratios and 95% CIs, compared with men using gels, injection initiators had higher hazards of cardiovascular events (ie, MI, unstable angina, and stroke) (1.26; 1.18-1.35), hospitalization (1.16; 1.13-1.19), and death (1.34; 1.15-1.56) but not VTE (0.92; 0.76-1.11). Compared with gels, patches did not confer increased hazards of cardiovascular events (1.10; 0.94-1.29), hospitalization (1.04; 1.00-1.08), death (1.02; 0.77-1.33), or VTE (1.08; 0.79-1.47).Testosterone injections were associated with a greater risk of cardiovascular events, hospitalizations, and deaths compared with gels. Patches and gels had similar risk profiles. However, this study did not assess whether patients met criteria for use of testosterone and did not assess the safety of testosterone among users compared with nonusers of the drug.
| S-EPMC4494981 | biostudies-literature