scholarly journals Development and validation of HPLC method for analysis of indolocarbazole derivative LCS-1269

Pharmacia ◽  
2021 ◽  
Vol 68 (2) ◽  
pp. 427-431
Author(s):  
Zoya Shprakh ◽  
Andrei Budko ◽  
Dmitry Kozin ◽  
Lydia Ektova ◽  
Dmitry Gusev ◽  
...  

Indolocarbazole glycosidic derivative LCS-1269 with significant antiproliferative activity has been synthesized in N.N. Blokhin National Medical Research Center of Oncology. To control the quality of the substance, the chromatographic method of the assay was created and validated. The technique was carried out in a gradient mode using mobile phases consist of acetonitrile, trifluoroacetic acid and purified water. The specificity of the method was shown by checking of test solutions and the special solvent chromatograms. The method linearity was confirmed, and the parameters of linear dependence have been estimated, and the relationship was described by the equation: y = 49.23× – 35.51 with correlation coefficient 0.9998. The method’s precision was determined as the repeatability with a relative error of the mean 1.49% and was 2.433 ± 0.036. Was shown, that the results obtained in the intermediate precision estimation were not burdened with a systematic error. The detection limit and quantitation limit were calculated based on the linear relationship data as 3.15 μg/mL and 9.57 μg/mL, respectively. Sensitive HPLC method for LCS-1269 assay in substance has been developed and validated.

2017 ◽  
Vol 1 (1) ◽  
pp. 44-49 ◽  
Author(s):  
Mariana Koetz ◽  
Thalita Gilda Santos ◽  
Magda Rayane ◽  
Amélia Teresinha Henriques

The leaves of Atropa belladonna (L) are characterized by the presence of the alkaloid atropine, known for the antimuscarinic activity. The leaves are used in therapy, mainly  in homeopathic preparations. An HPLC method was developed and validated to quantify atropine in belladonna leaves. The samples were extracted with methanol, followed by acid-base extraction with 5% HCl and dichloromethane. Analysis by HPLC was performed on C18 column, in a linear gradient system using a system with two mobile phases (water and acetonitrile), both acidified with trifluoroacetic acid. The determinations were performed using a reference standard and a diode array detector at 210 nm. The method was validated and proved to be specific / selective, comparing the UV profiles and the purity of the atropine peaks in reference and sample solutions and analyzing sample solutions with and without addition of standard, which produced an increase only of the area of peak of the sample, without changing the area of the adjacent peaks. The linearity (50 - 200 μg/mL) was provided by analysis of the analytical curves of atropine, with r2 = 0.9996. LOD and LOQ were 3.75 and 11.4 µg/ml, respectively. The method was precise, reproducible and accurate, and presented recovery equal to 103.0%. The method was considered robust for the analyzed parameters. Four commercial samples were analyzed and the mean levels of atropine found ranged from 0.16 - 0.27 %. Thus, the developed method is effective for quantification of atropine in beladona leaves and meets the validation requirements of current legislation and ensuring the quality control of the plant material.


2021 ◽  
Vol 8 ◽  
pp. 237437352110073
Author(s):  
Richard M Elias ◽  
Karen M Fischer ◽  
Mustaqeem A Siddiqui ◽  
Trevor Coons ◽  
Cindy A Meyerhofer ◽  
...  

Previous studies show that patient complaints can identify gaps in quality of care, but it is difficult to identify trends without categorization. We conducted a review of complaints relating to admissions on hospital internal medicine (HIM) services over a 26-month period. Data were collected on person characteristics and key features of the complaint. The complaints were also categorized into a previously published taxonomy. Seventy-six unsolicited complaints were identified, (3.5 per 1000 hospital admissions). Complaints were more likely on resident services. The mean duration between encounter and complaint was 18 days, and it took an average of 12 days to resolve the complaint. Most patients (59%) had a complaint in the Relationship domain. Thirty-nine percent of complaints mentioned a specific clinician. When a clinician was mentioned, complaints regarding communication and humaneness predominated (68%). The results indicate that the efforts to reduce patient complaints in HIM should focus on the Relationships domain.


2021 ◽  
Vol 80 (Suppl 1) ◽  
pp. 1079.1-1079
Author(s):  
I. Yoshii

Background:Boolean remission criteria is one most popular and stringent criteria in treating patient with rheumatoid arthritis (RA), because it may guarantees a stable clinical course after attaining remission.Objectives:Impact of time span from initiation to achieving Boolean remission on maintaining disease activity, daily activities, and quality of life after attaining Boolean remission was investigated from daily clinical practice data.Methods:685 patients with RA since August 2010 under the T2T strategy were treated. They were monitored for their TJC, SJC, PGA, EGA, CRP, and disease activity indices such as CDAI, SDAI, DAS28, and Boolean criteria at every visit. HAQ-DI score, pain score using visual analog scale (PS-VAS), and EQ-5D were also monitored, and the quality of life score (QOLS) calculated from EQ-5D was determined at every visit from the time of diagnosis (baseline).Of 685 patients, 465 patients had achieved Boolean remission >1 times, and were consecutively followed up for >3 years. These patients were enrolled in the study. Time span from the first visit to first Boolean remission was calculated. The relationship between the time span and each of background parameters, and the relationship between the time span and each of the mean values of the SDAI score, HAQ score, PS-VAS, SHS, and QOLS at the first Boolean remission and thereafter was evaluated statistically.Patients were subsequently divided into the G ≤ 6 and G > 6 groups based on the achievement of first Boolean remission within two groups: time span G ≤ 6 months and G > 6 months. The two groups were compared with regard to the SDAI score, HAQ score, PS-VAS, SHS, and QOLS at first visit and at the time of first Boolean remission, and the mean values of these parameters after remission were evaluated statistically. Moreover, changes of these parameters and the mean Boolean remission rate after the first remission, and SDAI remission rate at the first Boolean remission to thereafter were compared between the two groups statistically.Results:Out of 465 patients, females comprised 343 (73.7%), and the mean age was 67.8 years (range, from 21–95 years). The mean disease duration at first visit was 6.1 years (range, from 1 months–45 years). The mean follow up length was 88.1 months (range: 36–122 months; median: 85 months) and mean time span from the first visit to the first Boolean remission was 8.1 months. The mean SDAI score, HAQ score, PS-VAS, and the QOLS at first visit were 13.3, 0.467, 33.2, and 0.834, respectively. Among the study parameters, PS-VAS and QOLS were significantly correlated with the time span. For parameters at the first Boolean remission, HAQ-DI score, PS-VAS, and QOLS demonstrated significant correlation with the time span, whereas SDAI, HAQ-DI score, PS-VAS, SHS, and QOLS after the Boolean remission demonstrated significant correlation with the time span.The comparison between the G ≤ 6 and the G > 6 groups revealed that the disease duration, HAQ score, and PS-VAS at baseline in the G > 6 were significantly higher than that in the G ≤ 6 group, and QOLS in the G ≤ 6 group was significantly higher than that in the G > 6 group at baseline. Similarly, the HAQ score and PS-VAS at the first Boolean remission in the G > 6 group were significantly higher than that in the G ≤ 6 group, whereas QOLS in the G ≤ 6 group demonstrated no significant difference compared with that in the G > 6 group.The mean value of the SDAI score after the first Boolean remission in the G > 6 group was significantly higher than that in the G ≤ 6 group. Similarly, the SDAI score, HAQ score, and PS-VAS after the first Boolean remission in the G > 6 group were also significantly higher than those in the G ≤ 6 group, and the mean value of the QOLS in the G ≤ 6 group were significantly higher than that in the G > 6 group. The Boolean remission rate and SDAI remission rate after the first Boolean remission were significantly higher in the G ≤ 6 group than those in the G > 6 group.Conclusion:Attaining Boolean remission ≤ 6 months for RA has significant benefit for more stable disease control, that leads good maintenance of ADL.Disclosure of Interests:None declared


2021 ◽  
pp. 1-11
Author(s):  
Sultan M. Alshahrani ◽  
John Mark Christensen

This study was designed to develop and validate a simple and efficient high performance liquid chromatography (HPLC) method to determine flunixin concentrations in Asian elephant’s (Elephas maximus) plasma. Flunixin was administered orally at a dose of 0.8 mg/kg, and blood samples were collected. Flunixin extraction was performed by adding an equal amount of acetonitrile to plasma and centrifuging at 4500 rpm for 25 minutes. The supernatant was removed, and flunixin was analyzed using HPLC-UV detection. Two methods were developed and tested utilizing two different mobile phases either with or without adding methanol (ACN: H2O vs. ACN: H2O: MeOH). Both methods showed excellent linearity and reproducibility. The limit of detection was 0.05 ug/ml and limit of quantification was 0.1 ug/ml. the efficiency of flunixin recovery was maximized by the addition of methanol to mobile phase (ACN: H2O: MeOH as 50:30:20) at 95% in comparison to 23% without methanol. In conclusion, adding methanol to HPLC methods for extraction of flunixin from elephants’ plasma yielded higher recovery rate than without methanol.


2021 ◽  
Vol 28 (3) ◽  
pp. 384-394
Author(s):  
Kawoun Seo

Purpose: This study was done to investigate the mediating effects of acceptance action on the relationship between diabetes self-stigma and quality of life in diabetes patients.Methods: For this study a descriptive research approach was used. Patients (237) with a diagnosis of diabetes mellitus from a doctor of endocrinology were included. Data collection was done from March 26, to March 28, 2020. Data were analyzed using descriptive statistics, t-test, one-way ANOVA, Pearson’s correlation coefficient analysis, and hierarchecal multiple regression.Results: The mean scores for diabetes self-stigma, acceptance action and quality of life were 2.67±0.71, 4.12±0.38, and 3.26±0.48, respectively. Acceptance action was found to partial mediate the relationship between diabetes self-stigma and quality of life (z=-4.20, p<.001), and its explanatory power was 17.6%.Conclusion: To improve the quality of life among patients with diabetes in diabetes self-stigma situations, it is necessary to improve their acceptance action and develop step-by-step and differentiated acceptance action enhancement programs through multidisciplinary collaboration.


INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (04) ◽  
pp. 77-80
Author(s):  
M Vijaya Lakshmi ◽  
◽  
K Hima Bindu ◽  
M. Pravallika ◽  
B. N. Nalluri

A simple and precise RP-HPLC method has been developed and validated for the estimation of sarpogrelate hydrochloride, an anti-platelet drug in bulk and pharmaceutical dosage forms. Sarpogrelate is an antagonist at 5HT2A and 5HT2B receptors which blocks serotonin induced platelet aggregation and has application in the treatment of diseases including diabetes mellitus, Raynaud’s disease, angina pectoris and atherosclerosis. Chromatography was carried out on a Phenomenex C18 (250 x 4.6mm, 5μm) column with a mobile phase of 10mM ammonium acetate and acetonitrile (45:55% v/v). The flow rate was 1.2mL/min. The detection wavelength was carried out at 220nm. The retention time is 3.356 minutes for sarpogrelate hydrochloride. The linearity was found in the range of 10-50 μg/ml (R = 0.999) and % RSD is less than 2%. The mean recoveries obtained for sarpogrelate hydrochloride were in the range of 98.73-100.67%. The method is validated as per ICH guidelines and can be applied for the estimation of percentage purity in Sarpogrelate hydrochloride for quality control analysis in bulk and its dosage forms.


Circulation ◽  
2014 ◽  
Vol 130 (suppl_2) ◽  
Author(s):  
Karen Uzark ◽  
Cynthia Smith ◽  
Sunkyung Yu ◽  
Janet Donohue ◽  
Katherine Afton ◽  
...  

Objective: Transition is defined as “the process by which adolescents and young adults with chronic childhood illnesses are prepared to take charge of their lives and their health in adulthood”. We previously reported common knowledge deficits and lack of transition readiness (TR) in 13-25 year olds with congenital or acquired heart disease. The aims of this study were to re-evaluate TR in these patients at follow-up (F/U) and to examine the relationship between changes in TR and quality of life (QOL). Methods: Patients (n=106) completed the TR Assessment and Pediatric Quality of Life Inventory (PedsQL) utilizing an e-tablet, web-based format at a routine F/U clinic visit. Changes from initial to F/U scores were evaluated. Results: Median patient age was 18.7 yrs at a median F/U time of 1.02 yrs. Average perceived knowledge deficit score (% of items with no knowledge) at F/U was 18.0 ± 15.2%, decreased from 24.7 ± 16.5%, p<.0001. On a 100-point scale, the mean score for self-efficacy increased from 71.4 ± 17.0 to 76.7 ± 18.2 (p=.004) and for self-management increased from 47.9 ± 18.4 to 52.0 ± 20.7 (p=.0004). While physical QOL did not change, the mean psychosocial QOL score increased significantly from 80.2 ± 13.3 to 82.5 ± 12.0, p=.02. A decrease in knowledge deficit score at F/U was significantly associated with an increased psychosocial QOL score, p=.03. An increase in self-efficacy score was associated with an increase in psychosocial QOL score (p=.04), especially social QOL (p=.02). Among patients who reported receiving specific information after initial TR assessment, knowledge deficits decreased related to medication (p=.002), symptoms to call for (p=.02), how to contact heart doctor (p=.02), and health insurance (p=.10). Self-efficacy scores improved in patients reporting receipt of information regarding how to contact the heart doctor (p=.06) and how to communicate with healthcare team (p=.05). Conclusion: While deficits in knowledge and self-management skills persist, TR assessment and recognition of deficits can improve transition readiness with improved psychosocial QOL. Routine TR assessment is important to identify transition needs. Further studies are needed to examine the relationship between TR and outcomes in young adults with heart disease.


2018 ◽  
Vol 68 (2) ◽  
pp. 171-183
Author(s):  
Béla Kovács ◽  
Lajos Kristóf Kántor ◽  
Mircea Dumitru Croitoru ◽  
Éva Katalin Kelemen ◽  
Mona Obreja ◽  
...  

Abstract A reverse-phase HPLC (RP-HPLC) method was developed for strontium ranelate using a full factorial, screening experimental design. The analytical procedure was validated according to international guidelines for linearity, selectivity, sensitivity, accuracy and precision. A separate experimental design was used to demonstrate the robustness of the method. Strontium ranelate was eluted at 4.4 minutes and showed no interference with the excipients used in the formulation, at 321 nm. The method is linear in the range of 20–320 μg mL−1 (R2 = 0.99998). Recovery, tested in the range of 40–120 μg mL−1, was found to be 96.1–102.1 %. Intra-day and intermediate precision RSDs ranged from 1.0–1.4 and 1.2–1.4 %, resp. The limit of detection and limit of quantitation were 0.06 and 0.20 μg mL−1, resp. The proposed technique is fast, cost-effective, reliable and reproducible, and is proposed for the routine analysis of strontium ranelate.


2019 ◽  
Vol 24 (4) ◽  
pp. 655-663
Author(s):  
Ayla Hendekçi ◽  
Sonay Bilgin

This study was conducted to determine the quality of life and difficulties of adolescents in school age. This descriptive study was conducted in a city center three secondary School. Similarly from each school 114,114,116 people participated in the study, 4 students could not be included in the study due to insufficient data and the study was completed with 344 students. Questionnaire developed by the researcher, the Strengths and Difficulties Questionnaire (SDQ), and the Pediatric Quality of Life Inventory (PedsQL) were used for data collection. Research was completed in line with the ethical principles. According to the evaluations, it was observed that 50.6% of the students was 13 years old, 52% was male, and 53.5% was in the seventh grade. The total score average for PedsQL was 81.58 ± 13.65, and the mean total score for SDQ was 25.02 ± 4.813. A positive and significant correlation was found between “behavioral problems” subscale score of the SDQ and all subscales of PedsQL except the “physical health” subscale as well as the positive and significant correlation between the mean total scores of PedsQL and SDQ. It was observed that the quality of life of the students is affected negatively as the difficulties experienced during adolescence increase. Some recommendations were made to reveal the problems experienced by school-age adolescents and to increase their quality of life.


2018 ◽  
Vol 16 (2) ◽  
pp. 165-172 ◽  
Author(s):  
Asma Rahman ◽  
Mohammad Rashedul Haque ◽  
M Muhibur Rahman ◽  
Mohammad A Rashid

In the present study a rapid, accurate and precise chiral HPLC method was developed and validated for enantiomeric separation of racemate citalopram and escitalopram according to the guidelines of United States of Pharmacopeia (USP) and International Conference on Harmonization (ICH). The chiral chromatographic separation was achieved with ammonium acetate/ ethanol/ 2-propanol/ methylene dichloride (100 : 150 : 70 : 30, v/v) at a flow rate of 0.5 ml/min using a chiral CD-PH column. The HPLC analyses were monitored at 254 nm. The method showed a good linearity with regression coefficient (r2) of 0.998 in the range of 20.0-70.0 μg/ml for escitalopram. The detection limit (LOD), quantitation limit (LOQ) and average percentage of recovery for escitalopram were found to be 2.54, 7.68 μg/ml and 100.28% to 102.86%, respectively. The percentage of relative standard deviation (%RSD) for intra- and inter- day precision were found as 0.16% and 0.09%, respectively. The established method proved as reproducible with a %RSD value of less than 2 and having the robustness within specified limit. The present study also showed the enantiomeric purity or excess (%ee) of seven pharmaceutical preparations of escitalopram. Thus the proposed chiral method can be applied for the enantiomeric purity determination of escitalopram formulations.Dhaka Univ. J. Pharm. Sci. 16(2): 165-172, 2017 (December)


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