scholarly journals METHOD VALIDATION OF SIMVASTATIN IN PCL-PEG-PCL TRIBLOCK COPOLYMER MICELLES USING UV-VIS SPECTROPHOTOMETRIC FOR SOLUBILITY ENHANCEMENT ASSAY

Author(s):  
DEWI PATMAYUNI ◽  
T. N. SAIFULLAH SULAIMAN ◽  
ABDUL KARIM ZULKARNAIN ◽  
SHAUM SHIYAN

Objective: This study aims to increase the solubility of simvastatin (SIM), a hydrophobic drug, by incorporating it into PCL-PEG-PCL triblock copolymer micelles and validating the assay method used, namely Uv-Vis spectrophotometric. Methods: The shake flask method was used to determine the increase in solubility experienced by SIM after being incorporated into the micellar system. The values ​​of maximum wavelength (λmax), linearity, LOD, LOQ, accuracy, and precision were used as parameters measured to assess the validity of the assay method used. Results: The results showed that PCL-PEG-PCL triblock copolymer micelles could increase SIM solubility by 9.7 times (89.49±5.75 µg/ml) compared to SIM without modification (9.19±0.24 µg/ml). The validation results show the λmax value of 239 nm, a linear calibration curve with an R-value of 0.9994, LOD and LOQ of 0.33 µg/ml and 1.00 µg/ml, accurate measurement with recovery at concentrations of 80%, 100%, and 120% were 102.93±1.32%, 100.78±0.40%, and 104.58±0.79% and also had good precision ​​with RSD<2%. Conclusion: The PCL-PEG-PCL triblock copolymer micelles can increase SIM solubility and the Uv-Vis spectrophotometric method has been validated successfully for the quantitative analysis of SIM in PCL-PEG-PCL triblock copolymer micelles.

1973 ◽  
Vol 56 (3) ◽  
pp. 591-595
Author(s):  
Marshall A Malina

Abstract Four methods for the analysis of AG-chlordane and its formulations were submitted to a collaborative study. Fifteen laboratories, including 5 CIPAC laboratories, participated in this study. The infrared method for the analysis of the content of the 2 chlordane isomers was precise, with a coefficient of variation of 0.015. The gas chromatographic method for the analysis of the heptachlor content also yielded good precision with a standard deviation of 0.16. The infrared assay method for granular formulations exhibited excellent accuracy and precision, with a coefficient of variation of 0.067 and an error of only +0.25% relative. The gas chromatographic assay method for emulsifiable concentrates exhibited poor accuracy and precision and was found unacceptable. The first 3 methods have been adopted as official first action.


2011 ◽  
Vol 94 (6) ◽  
pp. 1758-1769 ◽  
Author(s):  
Abdel-Maaboud I Mohamed ◽  
Horria A Mohamed ◽  
Niveen M Abdel-Latif ◽  
Marwa R Mohamed

Abstract Two simple and sensitive spectrofluorimetric methods were developed for determination of three water-soluble vitamins (B1, B2, and B6) in mixtures in the presence of cyanocobalamin. The first one was for thiamine determination, which depends on the oxidation of thiamine HCl to thiochrome by iodine in an alkaline medium. The method was applied accurately to determine thiamine in binary, ternary, and quaternary mixtures with pyridoxine HCl, riboflavin, and cyanocobalamin without interference. In the second method, riboflavin and pyridoxine HCl were determined fluorimetrically in acetate buffer, pH 6. The three water-soluble vitamins (B1, B2, and B6) were determined spectrofluorimetrically in binary, ternary, and quaternary mixtures in the presence of cyanocobalamin. All variables were studied in order to optimize the reaction conditions. Linear relationship was obeyed for all studied vitamins by the proposed methods at their corresponding λexc or λem. The linear calibration curves were obtained from 10 to 500 ng/mL; the correlation ranged from 0.9991 to 0.9999. The suggested procedures were applied to the analysis of the investigated vitamins in their laboratory-prepared mixtures and pharmaceutical dosage forms from different manufacturers. The RSD range was 0.46–1.02%, which indicates good precision. No interference was observed from common pharmaceutical additives. Good recoveries (97.6 ± 0.7–101.2 ± 0.8%) were obtained. Statistical comparison of the results with reported methods shows excellent agreement and indicates no significant difference in accuracy and precision.


2019 ◽  
Vol 29 (3) ◽  
pp. 70
Author(s):  
Ruba Fahmi Abbas ◽  
Neda Ibrahim Mahdi ◽  
Ali Amer Waheb Amer Waheb ◽  
Amjad Gali Aliwi Gali Aliwi ◽  
Marwa S. Falih

Two Rapid, direct, ecological friendly and economical spectrophotometric methods were used for estimation of meloxicam in the market Tablet dosage form. The First method is based on the use the fourth order derivative spectrum (D4) and the second method is depend-ed on the ratio of the area under the curve for the two peaks in the drug (Compensated area under the curve). The linear calibration graphs of the two methods were measured in the con-centration range (5-35)mg/l and the average of recoveries for local market Tablet (AWA)® were 99.8% for D4 method and 100.2% for CAUC method which indicating a good accuracy and precision for these methods. In this study, the results obtained by these suggested meth-ods have been successfully statistically compared by t-test and Mann-Whitney test showed a good agreement.


2011 ◽  
Vol 94 (2) ◽  
pp. 467-481 ◽  
Author(s):  
Abdel-Maaboud I Mohamed ◽  
Horria A Mohamed ◽  
Niveen A Mohamed ◽  
Marwa R El-Zahery

Abstract Two spectrophotometric methods, derivative and multivariate methods, were applied for the determination of binary, ternary, and quaternary mixtures of the water-soluble vitamins thiamine HCl (I), pyridoxine HCl (II), riboflavin (III), and cyanocobalamin (IV). The first method is divided into first derivative and first derivative of ratio spectra methods, and the second into classical least squares and principal components regression methods. Both methods are based on spectrophotometric measurements of the studied vitamins in 0.1 M HCl solution in the range of 200500 nm for all components. The linear calibration curves were obtained from 2.590 g/mL, and the correlation coefficients ranged from 0.9991 to 0.9999. These methods were applied for the analysis of the following mixtures: (I) and (II); (I), (II), and (III); (I), (II), and (IV); and (I), (II), (III), and (IV). The described methods were successfully applied for the determination of vitamin combinations in synthetic mixtures and dosage forms from different manufacturers. The recovery ranged from 96.1 1.2 to 101.2 1.0 for derivative methods and 97.0 0.5 to 101.9 1.3 for multivariate methods. The results of the developed methods were compared with those of reported methods, and gave good accuracy and precision.


Author(s):  
DEWI PATMAYUNI ◽  
T. N. SAIFULLAH SULAIMAN ◽  
ABDUL KARIM ZULKARNAIN

Objective: This study aims to optimize PCL-PEG-PCL (PCEC) triblock copolymer micelles as a hydrophobic drug carrier, simvastatin (SV). Methods: PCEC triblock copolymer was prepared by the ring-opening polymerization method (ROP) with different ɛCL/PEG ratio (2 and 5). SV was incorporated into the PCEC triblock copolymer micelles with a concentration of 2.5 and 10 % w/w by the solvent evaporation method (film formation). The influence of the ɛCL/PEG ratio and concentration of SV effect on the responses particle size (PS), polydispersity index (PI) and entrapment efficiency (EE) was assessed using 22 full factorial design method. The test results were analyzed using Design-Expert software to obtain the optimum formula. Result: The selection of the optimum formula is based on the desirability value, the formula with the largest desirability value is chosen as the optimum formula. The results showed the optimum formula chosen had a desirability value of 0.860 consisting of a ɛCL/PEG ratio of 5 and SV concentration of 10 % w/w, with the PS, PI dan EE value was 322.1±3.51 nm, 0.471±0.09 and 87.08±1.17 %, respectively. Conclusion: The 22 full factorial design has been proven to be used as an optimization method to determine the optimum formula of SV-loaded PCEC triblock copolymer micelles with a good result of the PS, PI and EE responses.


RSC Advances ◽  
2015 ◽  
Vol 5 (26) ◽  
pp. 20025-20034 ◽  
Author(s):  
Yuling Li ◽  
Sai Wang ◽  
Dandan Zhu ◽  
Yuling Shen ◽  
Baixiang Du ◽  
...  

Reversibly shell cross-linked micelles based on a lipoic acid (LA) decorated triblock copolymer poly(ethylene glycol)-b-poly(γ-benzyl-l-glutamate)-b-poly(l-phenylalanine) have been developed for efficient intracellular delivery of DOX.


2011 ◽  
Vol 7 (10) ◽  
pp. 3700-3707 ◽  
Author(s):  
K. Van Butsele ◽  
M. Morille ◽  
C. Passirani ◽  
P. Legras ◽  
J.P. Benoit ◽  
...  

Author(s):  
Zeinab Adel Nasr ◽  
Noha S. Said ◽  
Sawsan A. Abdel-Razeq

Aims: Two spectrophotometric methods were developed and validated for the determination of sofosbuvir in presence of its alkaline degradate. Study Design: Ratio difference and ratio derivative methods were assisted for determination of sofosbuvir in presence of its alkaline degradate, laboratory-prepared mixtures and in tablet dosage forms. Place and Duration of Study: Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy (Girls), Al - Azhar University, between December 2019 and January 2020. Methodology: Two analytical methods were achieved and validated for the quantitative determination of Sofosbuvir in presence of its alkaline degradate. The first method was ratio difference (RD) method, where the UV absorption spectra of different concentrations of sofosbuvir were divided by the spectrum of a certain concentration (15 µg mL-1) as a devisor of its alkaline degradate to get the ratio difference spectra. Afterwards, the peak amplitudes difference between 253.7 and 243.5 nm were measured. The second method was the ratio derivative (1DR) method, where the first derivative of the ratio spectra (1DR) was obtained and its amplitude was measured at 247 and 268 nm. Good linearity was obtained over the concentration range of 3-15 µg mL-1 for the proposed methods. The proposed procedures were adopted for the selective determination of intact Sofosbuvir in presence of up to 80% of its degradation product. Sofosbuvir was exposed to different conditions as alkaline, acidic and oxidative degradation. Results: The proposed methods were developed and validated with good linearity range of 3-15 µg mL-1 for both methods, and also with good accuracy and precision. And the obtained results were statistically compared to those obtained by the reported method. Conclusion: Sofosbuvir was successfully determined by the proposed ratio difference and ratio derivative methods in bulk powder, laboratory prepared mixtures and tablet dosage form with good accuracy and precision. The methods were validated according to ICH guidelines. The results obtained were compared with those of the reported method and were found to be in good agreement.


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