scholarly journals Green and sensitive spectrofluorimetric method for the determination of two cephalosporins in dosage forms

2021 ◽  
Vol 8 (8) ◽  
pp. 210329
Author(s):  
Heba Abdel-Aziz ◽  
M. M. Tolba ◽  
N. El-Enany ◽  
F. A. Aly ◽  
M. E. Fathy

Using two green and sensitive spectrofluorimetric methods, we quantified two cephalosporins, cefepime (CFM) and cefazolin (CFZ), in raw and pharmaceutical formulations. The first method is based on the reaction between CFM and fluorescamine (borate buffer, pH 8), which yields a highly fluorescent product. After excitation at 384 nm, the fluorescent product emits light at 484 nm. At concentration ranges from 12.0 to 120.0 ng ml −1 , the relative fluorescence intensity/concentration curve was linear with a limit of quantification (LOQ) of 2.46 ng ml −1 . The second method relied on measuring the CFZ quenching action on acriflavine fluorescence through formation of an ion-associate complex using Britton–Robinson buffer at pH 8. We measured acriflavine fluorescence at 505 nm after excitation at 265 nm. The decrease in acriflavine fluorescence intensity was CFZ concentration-dependent. Using this method, we quantified CFZ in concentrations ranging from 1 to 10 µg ml −1 with a LOQ of 0.48 µg ml −1 . We studied and optimized the factors influencing reaction product formation. Moreover, we adapted our methods to the investigation of the mentioned drugs in raw and pharmaceutical formulations with greatly satisfying results. We statistically validated our methods according to International Council on Harmonisation Guidelines. The obtained results were consistent with those obtained with the official high-performance liquid chromatography methods.

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (05) ◽  
pp. 24-29
Author(s):  
V. K Parmar ◽  
◽  
H. R. Brahmbhatt

A simple, rapid and sensitive spectrofluorimetric method has been developed and validated for the determination of the non-ionic surfactant, polysorbate 80, from pharmaceutical formulation. The proposed method is based on a fluorescence enhancement of the probe (eosin B dye) with addition of polysorbate 80. The eosin B concentration was optimised and found to be 4μg/mL. The fluorescence intensity was measured in a diluting solvent, citric acid buffer (pH 4.0) using excitation and emission wavelengths, 545 nm and 580 nm, respectively. The fluorescence intensity was found to be liner over a concentration range of 16-80 μg/mL of polysorbate 80 with a high correlation coefficient (r = 0.9990). The developed method was validated in terms of linearity, precision, accuracy, limit of detection and limit of quantification and specificity. The limit of detection and limit of quantification for polysorbate 80 were found to be 2 μg/mL and 16 μg/mL, respectively. The developed method was successfully applied for the determination of polysorbate 80 in ophthalmic solution and micro emulsion.


2015 ◽  
Vol 2015 ◽  
pp. 1-9 ◽  
Author(s):  
Hany W. Darwish ◽  
Ahmed H. Bakheit ◽  
Ali Saber Abdelhameed ◽  
Amer S. AlKhairallah

An impressively simple and precise spectrofluorimetric procedure was established and validated for ponatinib (PTB) quantitation in biological fluids such as human plasma and human urine. This method depends on examining the fluorescence characteristics of PTB in a micellar system of Cremophor RH 40 (Cr RH 40). Cr RH 40 enhanced the intrinsic fluorescence of PTB distinctly in aqueous water. The fluorescence spectra of PTB was recorded at 457 nm following its excitation at 305 nm. Maximum fluorescence intensity was attained by addition of 0.7 mL of Cr RH 40 and one mL of phosphate buffer to PTB aliquots and then dilution with distilled water. There is a linear relationship between the fluorescence intensity of PTB and its concentration over the range 5–120 ngmL−1, with limit of detection and limit of quantification equal to 0.905 ngmL−1and 2.742 ngmL−1, respectively. The accuracy and the precisions of the proposed method were checked and gave adequate results. The adopted method was applied with a great success for PTB quantitation in different biological matrices (spiked human plasma and urine) giving high recovery values.


Molecules ◽  
2018 ◽  
Vol 23 (12) ◽  
pp. 3115 ◽  
Author(s):  
Alina Pyka-Pająk ◽  
Małgorzata Dołowy ◽  
Wioletta Parys ◽  
Katarzyna Bober ◽  
Grażyna Janikowska

A new, simple, and cost-effective TLC-densitometric method has been established for the simultaneous quantitative determination of acetylsalicylic acid and ascorbic acid in combined effervescent tablets. Separation was performed on aluminum silica gel 60F254 plates using chloroform-ethanol-glacial acid at a volume ratio of 5:4:0.03 as the mobile phase. UV densitometry was performed in absorbance mode at 200 nm and 268 nm for acetylsalicylic acid and ascorbic acid, respectively. The presented method was validated as per ICH guidelines by specificity, linearity, accuracy, precision, limit of detection, limit of quantification, and robustness. Method validations indicate a good sensitivity with a low value of LOD and LOQ of both examined active substances. The linearity range was found to be 1.50–9.00 μg/spot and 1.50–13.50 μg/spot for acetylsalicylic and ascorbic acid, respectively. A coefficient of variation that was less than 3% confirms the satisfactory accuracy and precision of the proposed method. The results of the assay of combined tablet formulation equal 97.1% and 101.6% in relation to the label claim that acetylsalicylic acid and ascorbic acid fulfill pharmacopoeial requirements. The developed TLC-densitometric method can be suitable for the routine simultaneous analysis of acetylsalicylic acid and ascorbic acid in combined pharmaceutical formulations. The proposed TLC-densitometry may be an alternative method to the modern high-performance liquid chromatography in the quality control of above-mentioned substances, and it can be applied when HPLC or GC is not affordable in the laboratory.


2011 ◽  
Vol 8 (4) ◽  
pp. 1958-1964 ◽  
Author(s):  
H. R. Prajapati ◽  
P. N. Raveshiya ◽  
J. M. Prajapati

A reversed phase high performance liquid chromatographic (RP–HPLC) method was developed and subsequently validated for the determination of atomoxetine hydrochloride in bulk and pharmaceutical formulation. The separation was done by a PerkinElmer Brownlee analytical C8 column (260 mm x 4.6 mm, 5 µm) using methanol: 50 mM KH2PO2buffer (PH adjusted to 6.8 with 0.1 M NaOH), 80:20 v/v as an eluent. UV detection was performed at 270 nm at a flow rate 1.0 mL/min. The validation of the method was performed, and specificity, reproducibility, precision accuracy and ruggedness were confirmed. The correlation coefficient was found to be 0.997 for atomoxetine hydrochloride. The recovery was in the range of 99.94 to 100.98% and limit of quantification was found to be 5.707 µg/mL. The method is simple, rapid, selective and economical too and can be used for the routine analysis of drug in pharmaceutical formulations.


2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Garima Balwani ◽  
Emil Joseph ◽  
Satish Reddi ◽  
Vibhu Nagpal ◽  
Ranendra N. Saha

A new, simple, rapid, sensitive, accurate, and affordable spectrofluorimetric method was developed and validated for the estimation of ganciclovir in bulk as well as in marketed formulations. The method was based on measuring the native fluorescence of ganciclovir in 0.2 M hydrochloric acid buffer of pH 1.2 at 374 nm after excitation at 257 nm. The calibration graph was found to be rectilinear in the concentration range of 0.25–2.00 μg mL−1. The limit of quantification and limit of detection were found to be 0.029 μg mL−1and 0.010μg mL−1, respectively. The method was fully validated for various parameters according to ICH guidelines. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2%) and can be successfully applied for the determination of ganciclovir in its commercial capsules with average percentage recovery of 101.31 ± 0.90.


2015 ◽  
Vol 11 (2) ◽  
pp. 3513-3531 ◽  
Author(s):  
Mona Elsayed Elshahed ◽  
Ibrahim Habib

A rapid, simple and highly sensitive spectrofluorimetric method is developed for the determination of Tamsulosin hydrochloride (Tams.HCl) in pharmaceutical formulations. The proposed method is based on investigation of the fluorescence spectral behavior of Tams.HCl in a sodium dodecyl sulphate (SDS) micellar system. In aqueous solution of Tris buffer of pH 7±0.2, SDS causes marked enhancement in the fluorescence intensity of Tams.HCl (about +110%). The fluorescence intensity is measured at 328 nm after excitation at 280 nm and the fluorescence-concentration plots are rectilinear over the range 0.1-1.2 µg ml-1, with lower detection limit of 0.027 µg ml-1 and quantification limit of 0.09 µg ml-1. The method is successfully applied to the analysis of the studied drug in its commercial capsules, and the results are in good agreement with those obtained with the official method. The application of the proposed method is extended to stability studies of Tamsulosin hydrochloride after exposure to different forced degradation conditions, such as acidic, alkaline and oxidative conditions, according to ICH guidelines.


2011 ◽  
Vol 8 (s1) ◽  
pp. S304-S308 ◽  
Author(s):  
V. Rajesh ◽  
V. Jagathi ◽  
K. Sindhuri ◽  
G. Devala Rao

A simple and sensitive spectrofluorimetric method has been developed for the estimation of erlotinib hydrochloride in pure and pharmaceutical dosage forms. Erlotinib hydrochloride exhibits maximum fluorescence intensity in methanol and the Beer's law was obeyed in the range of 1-5 µg/mL at an excitation wavelength (λex) of 295 nm and an emission wavelength (λem) of 339 nm. Stability studies with respect to time and temperature were also carried out. The results obtained were in good agreement with the labelled amounts of the marketed formulations. This method has been statistically evaluated and found to be accurate and precise.


2013 ◽  
Vol 2013 ◽  
pp. 1-7
Author(s):  
Safwan Ashour ◽  
Nuha Kattan

A sensitive and precise RP-HPLC method has been developed for the simultaneous estimation of clidinium bromide (CDB) and chlordiazepoxide (CDZ) in pure and pharmaceutical formulations. The separation was achieved on a Nucleodur C8 ( mm i.d., 5 μm particle size) column at 25°C. CH3CN-MeOH-NH4OAc 0.1M (30 : 40 : 30, v/v/v) was used as the mobile phase at a flow rate of 1.0 mL min−1 and detector wavelength at 218 nm. Almotriptan (ALT) was used as internal standard. The validation of the proposed method was carried out for linearity, accuracy, precision, LOD, LOQ, and robustness. The method showed good linearity in the ranges of 2.5–300.0 and 3.0–500.0 μg mL−1 for CDB and CDZ, respectively. The percentage recovery obtained for CDB and CDZ was 100.40–103.38 and 99.98–105.59%, respectively. LOD and LOQ were 0.088 and 0.294 μg mL−1 for CDB and 0.121 and 0.403 μg mL−1 for CDZ, respectively. The proposed method was successfully applied to the determination of CDB and CDZ in combined dosage forms and the results tallied well with the label claim.


2010 ◽  
Vol 46 (2) ◽  
pp. 281-287 ◽  
Author(s):  
Amarilis Scremin ◽  
Monika Piazzon ◽  
Marcos Antonio Segatto Silva ◽  
Gislaine Kuminek ◽  
Giane Márcia Correa ◽  
...  

Deflazacort (DFZ) is a glucocorticoid used as an anti-inflammatory and immunosuppressant drug. No official methods are available for DFZ determination in pharmaceutical formulations. The objective of this study was to develop, validate and compare spectrophotometric (UV and colorimetric) and high-performance liquid chromatography (HPLC) methods, for the quantitative determination of DFZ in tablets and oral suspension. For the UV method, ethanol was used as the solvent, with detection at 244 nm. The colorimetric method was based on the redox reaction with blue tetrazolium in alkaline medium, with detection at 524 nm. The method by HPLC was carried out using a C18 column, mobile phase consisting of acetonitrile:water (80:20, v/v) with a flow rate of 1.0 mL min-1 and detection at 244 nm. The methods proved linear (r > 0.999), precise (RSD < 5%) and accurate (recovery > 97%). Statistical analysis of the results indicated that the UV and HPLC methods were statistically equivalent, while the values obtained for the colorimetric method differed significantly from the other methods.


Author(s):  
Mohammad Mojeeb Gulzar Khan ◽  
Pawar Vivek Laxman ◽  
Abdul Talib ◽  
Sandip Dinkar Firke ◽  
Mohan G Kalaskar ◽  
...  

For the determination of pimvanserin tartrate in bulk and formulation, a rapid and simple High Performance Thin Layer Chromatography at 226 nm was developed and validated. The determination was carried out on thin coated aluminum backing plates covered with 200 mm layer of silica gel G 60 F254 (10×10 cm) plate as stationary phase and using a mobile phase of methanol: chloroform: trimethylamine (4:6:0.1 v/v/v) respectively. With a correlation coefficient (r) of 0.998, the development of pimvanserin tartrate was linear in the range of 0.7 to 4.2 µg/ml. The limit of detection (LOD) was found to be 7.68 ng/spot while the limit of quantification was found to be 23.28 ng/spot. The percentage label claim of pimvanserin tartrate in bulk and formulation was found to be 99 – 101 %. The percentage found in the formulation shows that no effect of excipient on drug. The conducted procedure has the benefit of being simple and quick. As a result, it can be used to examine pimvanserin tartrate in pharmaceutical formulations.


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