Development and Validation of a Sensitive Spectrofluorimetric Method for the Determination of Ibrutinib (original) (raw)
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Asian Journal of Pharmaceutical and Clinical Research, 2018
Objective: Knowing the exact amount of active pharmaceutical ingredient (API) in pharmaceutical dosage form is of utmost importance to meet regulatory requirements and to ensure patient safety. Spectrophotometric analysis provides a simple, efficient, and economic approach for estimation of API in the pharmaceutical dosage form. In the present work, we have developed simple, sensitive, and highly economic ultraviolet (UV) spectrophotometric method for the estimation of amoxapine in a pharmaceutical formulation. Methods: Amoxapine shows maximum absorbance of light at wavelength 297 nm in water. The linearity study revealed that it obeys Beer-Lambert's law over the range of 2-20 µg/mL. Absorptivity value of amoxapine was found to be 206.6±1.341. Result: The tablet formulation was successfully analyzed by developed UV spectrophotometric method. The developed method was validated as per International Conference on Harmonization guidelines with respect to accuracy, precision, specificity robustness. The limit of detection and limit of quantitation was found to be 19.8 and 60.50 ng/mL, respectively. Conclusion: The developed method is simple, precise, accurate, and cost-effective and can be used for routine analysis of amoxapine.
Spectrofluorimetric determination of amlodipine in human plasma without derivatization
Brazilian Journal of Pharmaceutical Sciences, 2012
A rapid and sensitive spectrofluorimetric method was developed for the determination of amlodipine (AD), a calcium channel blocker, in the plasma. The type of solvent, the wavelength range, and the range of AD concentration were selected to optimize the experimental conditions. The calibration curves were linear (r² >0.997) in the concentration range of 0.1-12.5 ppm of AD. The limit of quantitation and limit of detection values for the method for plasma samples were 0.1 ppm and 0.07 ppm, respectively. The precision calculated as the relative standard deviation was less than 3.5%, and the accuracy (relative error) was better than 5.5% (n=6). The method developed in this study can be directly and easily applied for the determination of AD in the plasma without derivatization in plasma.
Journal of Chromatography B: Biomedical Sciences and Applications, 2001
This study compares HPLC electrospray time-of-flight mass spectrometry and selected reaction monitoring (SRM) LC-MS for high throughput quantitative determination of a small molecule drug in biological samples. A high throughput LC-MS method was developed for quantitatative determination of idoxifene in human plasma and the evaluation was accomplished with the cross-validation of the developed LC-MS method between the time-of-flight mass spectrometer, and a triple quadrupole mass spectrometer operated in the SRM mode. A simple one-step semi-automated 96-well liquid-liquid extraction procedure was used to prepare 96 samples in approximately 30 min and a rapid gradient was used to shorten the LC run time. Time-of-flight mass spectrometry provides acquisition of full-scan mass spectra and extracted ion current chromatograms, which may be extracted from the total ion current chromatogram for peak area determination. The limit of quantitation for idoxifene in human plasma obtained with the time-of-flight mass spectrometer was 5 ng / ml based on 100-ml aliquots of human plasma, and the linear dynamic range was from 5 ng / ml to 2000 ng / ml. The quantitative LC-MS results from the time-of-flight mass spectrometer demonstrated that precision did not exceed 7.1% and accuracy did not exceed 1.7% with reference to quality control samples at three concentration levels in replicates of six. In contrast, the limit of quantitation for idoxifene in human plasma using a tandem triple quadrupole mass spectrometer was 0.5 ng / ml with a linear dynamic range to 1000 ng / ml. The results from the triple quadrupole instrument show that the precision did not exceed 2.2% and accuracy did not exceed 2.9%. The overall results suggest time-of-flight mass spectrometry may be a viable technique for high throughput bioanalytical work for the quantitative determination of a representative small molecule drug in the low ng / ml range in human plasma.
A new spectrofluorimetric approach for the quantitation of imipramine HCl in commercial dosage forms
Journal of Advanced Pharmaceutical Science And Technology, 2017
A spectrofluorimetric method has been developed for the determination of imipramine HCl in bulk and commercial dosage forms. The method was based on measuring the fluorescence emission intensity of imipramine-eosin Y ion pair complex (λ em = 558 and λ ex = 319) in dichloroethane at buffer solution (sodium acetate and acetic acid) of pH 4.8. The stoichiometric ratio between imipramine and eosin Y was studied by Job's method of continuous variations and found to be 2:1. Formation constant (K f) and Gibb's free energy change (ΔG) were calculated and pointed towards the spontaneous nature of the reaction. A series of variables were studied to optimize the reaction conditions. The proposed method was validated as per ICH guidelines and successfully applied for the determination of active imipramine HCl in commercial dosage forms with high degree of accuracy and precision.
Two new simple, selective economical and reproducible UV spectrophotometeric method simultaneous estimation of two component drug mixture of Amlodipine besylate (AB)) and hydrochlorothiazide (HCT) in pharmaceutical preparation, blood sample and urine has been developed. The first method depends on first derivative method at 245 and 238 nm for AB and HCT also in plasma and urine respectively. The linearity over the concentration ranges 2.5-17.5µg/ml for both the drugs AB and HCT. The second method is based on two wavelength method, which uses the difference of absorbance value at 271 nm and 395 nm for estimation of Hydrochlorothiazide (HCT) and absorbance at 363 nm for amlodipine besylate (AB). In formulation, plasma and urine Methanol: water (50:50v/v) was used as solvent, in which Amlodipine besylate and Hydrochlorothiazide shows linearity in the range of 2.5-17.5 µg/ml for both the drugs respectively. Standard deviation was <1.5 in the assay of tablets. This method validated an...
Chemical Papers
For quantitation of amlodipine (AML) and perindopril (PER) in their authentic, pharmaceutical formulations and spiked human plasma, a simple, sensitive, validated and inexpensive spectrofluorimetric method has been developed. The proposed method is developed to be based on quantitative quenching effect of two antihypertensive drugs on Eosin Y's native fluorescence which was achieved by developing binary complexes between each of the cited drugs in an acidic environment using acetate buffer (pH 4.4) with Eosin Y. Fluorescence quenching was recorded at 544 nm after excitation at 425 nm. For AML and PER, calibration curves were obtained over the range of 0.3–3.0 µg/mL and 0.2–2.0 µg/mL, respectively, with correlation coefficients of 0.9993 and 0.9995, respectively. The developed method was validated according to ICH guidelines. The proposed spectrofluorimetric method is regarded new and sensitive. As a result, the proposed method might be used to estimate the quality of the cited d...
Chemical Papers, 2010
Simple and rapid spectrophotometric methods have been developed for the microdetermination of fluoxetine HCl. The proposed methods are based on the formation of ion-pair complexes between fluoxetine and bromophenol blue (BPB), bromothymol blue (BTB), bromocresol green (BCG), and bromocresol purple (BCP) which can be measured at optimum λmax. Optimization of reaction conditions was investigated. Beer's law was obeyed in the concentration ranges of 0.5-8.0 µg mL −1 , whereas optimum concentration as adopted from the Ringbom plots was 0.7-7.7 µg mL −1 . The molar absorptivity, Sandell sensitivity, and detection limit were also calculated. The most optimal and sensitive method was developed using BCG. The correlation coefficient was 0.9988 (n = 6) with a relative standard deviation of 1.25, for six determinations of 4.0 µg mL −1 . The proposed methods were successfully applied to the determination of fluoxetine hydrochloride in its dosage forms and in biological fluids (spiked plasma sample) using the standard addition technique.
A new, simple, accurate, precise and reproducible UV spectrophotometric method is being developed for the simultaneous estimation of amlodipine besylate, olmesartan medoxomil and hydrochlorthiazide in tablet dosage form. The stock solutions were prepared in methanol. The λ max for amlodipine besylate, olmesartan medoxomil and hydrochlorthiazide were 238.5nm, 256.5nm and 271.5nm respectively. The amlodipine besylate, olmesartan medoxomil and hydrochlorthiazide obeyed Beer's law in concentration range of 5-25µg/ml, 6-30µg/ml and 5-25µg/ ml respectively. Results of analysis of simultaneous equation method were analyzed and validated for various parameters according to ICH guidelines.
Uv Spectrophotometric Methods for the Simultaneous Determination of Amoxicillin and Flucloxacillin
Al-Azhar Journal of Pharmaceutical Sciences
Spectrophotometric methods were introduced for the simultaneous determination of Amoxicillin (AMX) and flucloxacillin(FLX) in their pure forms and capsules pharmaceutical formulations. The first method was ratio difference (RD), in which the amplitude difference between 238 and 255 nm for AMX and between 254 and 238 nm for FLX were measured.The second one was mean centering of ratio spectra (MCR) in which the peak amplitude at 286nm for the determination of AMX and the peak amplitude at 236 nm for the estimation of FLX were measured. The third method was Area under the curve (AUC) where the range of 226 and 236 nm were adopted for AMX determination and of 240 and 247 nm for FLX determination. All of the previous methods were successfully used for quantitation of AMX and FLX in concentration ranges of 5-50µg/ml and 10-70µg/ml, respectively by RD and MCR methods and of 10-60µg/ml and 10-70µg/ml, respectively for AMX and FLX by AUC method. All of the developed methods were validated using ICH guidelines and statistically compared to a reported method. The adopted methods can be applied for the regular analysis of AMX and FLX mixture in QC laboratories.
Analytical Chemistry Letters, 2016
A UV-spectrophotometric and stability-indicating RP-HPLC method was developed and validated for concurrent estimation of Amlodipine besylate (AMDB) and Indapamide (INDA) in combined tablet dosage form in the presence of degradation products generated from stress degradation studies. For the RP-HPLC; Chromatography was carried on Shimadzu LC-20AT series HPLC; C-18 ODS bonded column (25cm × 4.60 mm, 10 μl, 40°C) used as stationary phase; methanol: water (95:5 % v/v) as mobile phase. The retention time of the AMDB and INDA were 8.780 and 2.850 min, respectively; detection at λ max 238 nm for both of drug (overlain spectra). Linear regression analysis shows a good linear relationship; in the concentration range of 2-16 μg/ml and 1-7 μg/ml; for AMDB and INDA with r > 0.999. These methods were accurate with a relative standard deviation of less than 2 % for both drugs. Stress conditions like acid, alkali degradation, hydrolytic, thermal and oxidation were applied and quantify by the RP-HPLC method. The degradation products did not interfere with the detection of AMDB and INDA, thus the method can be considered as a stabilityindicating method. The UV-spectrophotometric simultaneous equation method was based on the measurement of absorbance at two wavelengths; the λ max for AMDB and INDA was found to be 237 & 242 nm respectively for analytical measurement. The drugs AMDB and INDA follow the Beer's law in the concentration range of 5-25 μg/ml and 1-11 μg/ml, respectively; showing correlation coefficient (r) of 0.9980 for AMDB and 0.9990 for INDA. These methods were successfully applied for reliable quantification of AMDB and INDA in commercial and routine analysis in combined dosage form.