Spectroscopic Fingerprinting of Aminoglycosides and Determination of Neomycin Sulphate Through Oxidative Ion-pair Complex Formation using Ammonium Molybdate

2019 ◽  
Vol 15 (5) ◽  
pp. 487-496 ◽  
Author(s):  
Edebi Nicholas Vaikosen ◽  
Benjamin Umar Ebeshi ◽  
Chimenem Ruth Worlu
Keyword(s):  
Regression Coefficient ◽  
Limit Of Detection ◽  
Ion Pair ◽  
Ammonium Molybdate ◽  
Official Method ◽  
Limit Of Quantification ◽  
Indirect Determination ◽  
Spectrophotometric Methods ◽  
Assay Methods

Background:Aminoglycosides are non-chromophoric antibiotics. The official method of assay in pharmacopoeias is microbiological. Bioassay methods are potency-semi-quantitative, laborious and time-consuming. In contrast, spectrophotometric methods are rapid, convenient, specific, sensitive and selective. The presence of NH2 and -OH functional groups in aminoglycosides makes them susceptible to redox reaction.Objective:A simple, cheap, quick, accurate and reliable spectrophotometric method for aminoglycoside analysis using neomycin as prototype via oxidation by ammonium molybdate reagent is proposed.Methods:Four aminoglycosides - amikacin, gentamicin, neomycin and streptomycin, were oxidized using ammonium molybdate (pH<2). These were scanned to obtain visible-spectrophotometric fingerprints. Two assay methods were developed. Method I involved the determination of the drug via the linear proportionality between neomycin and residual molybdate measured at 780nm and 850nm. Method II, an indirect determination using ion-pair reaction of excess molybdate and methyl orange measured at 430nm and 480nm.Results:All aminoglycosides formed blue complex, with distinct spectra peaks at 500nm, 640nm, 780nm and 850nm.The limit of detection and limit of quantification were from 0.33 to 2.32 μgmL-1 and 1.00 to 7.03 μgm L-1 respectively for both methods. Percentage recoveries ranged from 89.60 and 113.05 %, while precision and accuracy as RSD ranged from 0.23 to 3.55%. The regression coefficient (R2) ranged from 0.9968 to 0.9995. Percentage neomycin in dosage forms ranged from 95.67- 104.16% and 96.04 - 99.46% for methods I and II, respectively.Conclusion:The methods were successfully applied for neomycin sulphate determination in tablets and drops, therefore aminoglycosides could be assayed via the proposed methods.

scholarly journals Determination of bisphenol a in baby bottles and drinking containers by high liquid chromatography

2019 ◽  
pp. 332-337
Author(s):  
Gorica Vukovic ◽  
Marina Djukic ◽  
Tijana Stojanovic ◽  
Vojislava Bursic ◽  
Aleksandra Petrovic ◽  
...  
Keyword(s):  
Bisphenol A ◽  
Digital Media ◽  
Epoxy Resins ◽  
Regression Coefficient ◽  
Limit Of Detection ◽  
Protective Coatings ◽  
Limit Of Quantification ◽  
Baby Bottles ◽  
Food And Drink

Bisphenol A is a monomer used primarily in the production of polycarbonate plastics and epoxy resins. Polycarbonate plastic is used in a wide variety of digital media products, electrical and electronic equipment, sport safety equipment, reusable food and drink containers, etc. Epoxy resins are used in engineering applications, paints and adhesives and also in a variety of protective coatings in metal cans for foods, bottle tops and water supply pipes. The content of BPA was evaluated in 16 samples (6 baby bottles and 10 drinking containers - can) collected during 2018/2019, of which three baby bottles and 8 cans were collected in 2018, while three baby bottles and 2 cans in 2019. A simple HPLC-FLD analytical method was validated for the quantitation of BPA from baby feeding bottles and cans. The separation was performed on a C18 column. Good linearity was obtained over the concentration range of 0.3-6.0 ?g/mL with the regression coefficient (R2) of 0.9998. The limit of detection (LOD) and limit of quantification (LOQ) were 0.01 and 0.03 ?g/mL, respectively. The repeatability of the method (%RSD) was between 4 and 6%, while the recovery ranged from 104.3 to 109.7%. The extraction of BPA was done in accordance with SRPS EN 13130-1:2008. The methods were applied to determine BPA release from baby bottles, performing repeated procedures according to EU and national regulations (SRPS CEN/TS 13130-13 (2008)). The conformity was evaluated according to National and EU requirements. The results show that Bisphenol-A was not detectable in any of the analysed samples.

scholarly journals HPLC-UV Determination of Dextromethorphan in Syrup Method validation

2019 ◽  
Vol 70 (2) ◽  
pp. 487-490
Author(s):  
Nicolae Avram ◽  
Simona Codruta Heghes ◽  
Luca-Liviu Rus ◽  
Anca Maria Juncan ◽  
Lucia Maria Rus ◽  
...  
Keyword(s):  
Ammonium Nitrate ◽  
Flow Rate ◽  
Chromatographic Analysis ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Ion Pair ◽  
Limit Of Quantification ◽  
System Suitability ◽  
Dextromethorphan Hydrobromide

A HPLC-UV method, for determination of dextromethorphan hydrobromide in syrup, was validated. The chromatographic analysis was performed using an RP-18, Nucleodur chromatographic column (250 mm � 4 mm, 5 �m) at constant temperature (50oC) with a mobile phase consisting of a mixture of acetonitrile/methanol (70:30 v/v) with sodium docusate (as ion pair agent) and ammonium nitrate, pH = 3.4. The flow rate of the mobile phase was 1 mL/min and the detection was carried out at 280 nm. System suitability, specificity, linearity, precision, accuracy, limit of detection and limit of quantification agreed with current pharmacopeial requests. The method is suitable for routine analysis of dextromethorphan hydrobromide in syrup.

scholarly journals Extractive Spectrophotometric Determination of Nortriptyline Hydrochloride Using Sudan II, IV and Black B

2001 ◽  
Vol 69 (2) ◽  
pp. 151-160
Author(s):  
A. Amin ◽  
H. Saleh
Keyword(s):  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Ion Pair ◽  
Calibration Graph ◽  
Official Method ◽  
Spectrophotometric Methods ◽  
Sudan Black B ◽  
Relative Standard ◽  
Nortriptyline Hydrochloride

A simple spectrophotometric methods has been developed for the determination of nortriptyline hydrochloride in pure and in pharmaceutical formulations based on the formation of ion-pair complexes with sudun II (SII), sudan (IV) (SIV) and sudan black B (SBB). The selectivity of the method was improved through extraction with chloroform. The optimum conditions for complete extracted colour development were assessed. The absorbance measurements were made at 534, 596 and 649 nm for SII, SIV and SBB complexes, respectively. The calibration graph was linear in the ranges 0.5- 280. 0.5- 37.5 and 0.5 – 31.0 μg ml−1 of the drug usiny the same reagents, respectively. The precision of the procedure was checked by calculating the relative standard deviation of ten replicate determinations on 15 μg ml−1 of nortriptyline HCI and was found to be 1.7, 1.3 and 1.55% using SII, SIV, and SBB complexes, respectively. The molar absorptivity and Sandell sensitivity for each ion-pair were calculated. The proposed methods were successfully applied to the deterniination of pure nortriptyline HCI and in pharmaceutical formulations, and the results demonstrated that the method is equally accurate, precise and reproducible as the official method.

scholarly journals ANALYTICAL METHOD VALIDATION OF ICP-AES FOR ANALYSIS OF CADMIUM, CHROMIUM, CUPRUM, MANGAN AND NICKEL IN MILK

2019 ◽  
pp. 341-344
Author(s):  
DAVID ALEXANDER ◽  
Abdul Rohman
Keyword(s):  
Heavy Metals ◽  
Analytical Method ◽  
Limit Of Detection ◽  
Official Method ◽  
Fast Method ◽  
Limit Of Quantification ◽  
Milk Products ◽  
Relative Standard ◽  
Validation Parameters

Objective: The aim of this research was to validate inductively coupled plasma-atomic emission spectroscopy (ICP-AES) for quantitative analysis of cadmium (Cd), chromium (Cr), cuprum (Cu), mangan (Mn) and nickel (Ni) in milk products. Methods: The heavy metals in milk were determined using ICP-AES at optimized wavelength. The method was validated by assessing several validation parameters which included linearity and range, accuracy, precision and sensitivity expressed by the limit of detection and limit of quantification. The validated method was then used for the analysis of milks commercially available. Results: ICP-AES for determination of Cd, Cr, Cu, Mn, and Ni was linear over a certain concentration range with a coefficient correlation value of>0.997. The limit of quantification values of Cd, Cr, Cu, Mn, and Ni were 0.0047; 0.0050; 0.0066; 0.0061; and 0.0169 µg/ml, respectively. The precision of analytical method exhibited relative standard deviation (RSD) values of 3.18%; 4.17%; 3.05%; 2.93%; and 4.47% during repeatability test and 5.28%; 5.06%; 3.67%; 3.67%; and 11.17% during intermediate precision of Cd, Cr, Cu, Mn, and Ni respectively. The recoveries of these metals assessed using standard addition method were 92.25; 90.88; 102.87; 94.50; and 86.85%, respectively. Conclusion: ICP-AES offered a reliable and fast method for the determination of heavy metals in milk products. The developed method could be proposed as an official method for determination of heavy metals in milk products.

scholarly journals Of bromination reaction for the spectrophotometric assay of domperidone in pharmaceuticals

2011 ◽  
Vol 17 (1) ◽  
pp. 81-89 ◽  
Author(s):  
Zenita Devi ◽  
K. Basavaiah ◽  
K.B. Vinay
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Reference Method ◽  
Standard Addition ◽  
Limit Of Quantification ◽  
Fixed Amount ◽  
Spectrophotometric Methods ◽  
Significant Difference ◽  
Bulk Drug

Three simple and sensitive spectrophotometric methods are described for the determination of domperidone (DOM) in bulk drug and in dosage forms using bromate-bromide mixture as brominating agent in acid medium and three dyes, meta-cresol purple (MCP), amaranth (AMR) and erioglaucine (EGC). The methods involve the addition of a known excess of bromate-bromide mixture to an acidified solution of DOM followed by the determination of the residual bromine by reacting with a fixed amount of either MCP dye and measuring the absorbance at 530 nm (method A) or AMR dye and measuring the absorbance at 520 nm (method B) or EGC dye and measuring the absorbance at 630 nm (method C). Beer?s law is obeyed over the concentration ranges, 0.63 - 10.0, 0.25-4.0 and 0.13-2.0 ?g mL-1 for method A, method B and method C, respectively. The apparent molar absorptivities are calculated to be 3.751 ? 104, 6.604 ? 104 and 1.987 ? 105 L mol-1cm-1 for method A, method B and method C, respectively and the corresponding sandell sensitivity values are 0.011, 0.006 and 0.002 ?g cm-2. The limit of detection and the limit of quantification are also reported for all the three methods. No interference was observed from common additives found in pharmaceutical preparations. Statistical comparisons of the results with those of the reference method showed an excellent agreement, and indicated no significant difference in accuracy and precision. The accuracy and reliability of the methods were further ascertained by performing recovery tests via standard-addition technique.

scholarly journals Extractive spectrophotometric determination of Quetiapine fumarate in pharmaceuticals and human urine using calmagite as an ion-pair reagent

2011 ◽  
Vol 17 (3) ◽  
pp. 259-267 ◽  
Author(s):  
Nagaraju Rajendraprasad ◽  
Kanakapura Basavaiahf ◽  
Basavaiah Vinay
Keyword(s):  
Human Urine ◽  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Ion Pair ◽  
Official Method ◽  
Quetiapine Fumarate ◽  
Relative Standard ◽  
Significant Difference ◽  
Comparison Of The Results

Quetiapine fumarate (QTF) is an antipsychotic drug belonging to the benzisoxazole derivatives indicated for the treatment of schizophrenia. A sensitive and selective method based on dichloromethane-extractable ion-pair of QTF with calmagite (CGT), which exhibited an absorption maximum at 490 nm, is described. At this wavelength, Beer?s law is obeyed over the concentration range of 3.0 - 30.0 ?g ml-1. The apparent molar absorptivity, limit of detection (LOD) and quantitation (LOQ) values are 1.32 ? 104 l mol-1 cm-1, 0.27 and 0.81 ?g ml-1 respectively. The reaction is extremely rapid at room temperature and the absorbance values remain unchanged upto 19 h. The precision results, expressed as intra-day and inter-day relative standard deviation values, are satisfactory (RSD ? 2.2%). The accuracy is satisfactory as well (RE ? 2.44%). The method was successfully applied to the determination of QTF in pharmaceuticals and spiked human urine with satisfactory results. No interference was observed from common pharmaceutical adjuvants in tablets. Statistical comparison of the results with official method showed an excellent agreement and indicated no significant difference in precision.

scholarly journals DEVELOPMENT AND VALIDATION OF NEW SPECTROPHOTOMETRIC METHODS FOR ESTIMATION OF ANTIPSYCHOTIC DRUG ASENAPINE MALEATE IN PURE AND DOSAGE FORMS

2020 ◽  
pp. 62-69
Author(s):  
RAGAA EL-SHEIKH ◽  
AHLAM E. ABD ELLATEIF ◽  
ESRAA AKMAL ◽  
AYMAN A. GOUDA
Keyword(s):  
Limit Of Detection ◽  
Dosage Forms ◽  
Ion Pair ◽  
Stoichiometric Ratio ◽  
Bromocresol Purple ◽  
Pharmaceutical Dosage Forms ◽  
Spectrophotometric Methods ◽  
Accuracy And Precision ◽  
Significant Difference

Objective: Three sensitive, simple, precise, reproducible, and validated spectrophotometric methods have been developed for the determination of anti-psychotic drug (asenapine maleate) in pure and pharmaceutical dosage forms. Methods: The methods are based on the formation of yellow-colored ion-pair complex between asenapine maleate and three acid dyes, namely, bromocresol purple (BCP), bromophenol blue (BPB) and bromothymol blue (BTB) with absorption maxima at 410, 414 and 416 nm, respectively. Several parameters such as pH, buffer type and volume, reagent volume, the sequence of addition and effect of extracting solvent were optimized. Results: Under the optimum experimental conditions, beer’s law is obeyed over the concentration ranges of 1.0–20, 1.0–14, and 1.0-16 μg/ml for BCP, BPB and BTB, respectively, with good correlation coefficients (0.9994-0.9998). The apparent molar absorptivity and Sandell’s sensitivity values are reported for all methods. The limit of detection (LOD) and the limit of quantification (LOQ) values are found to be 0.27, 0.30, and 0.25 μg/ml and 0.90, 1.0, and 0.83 μg/ml for BCP, BPB and BTB, respectively. The stoichiometric ratio of the formed ion-pair complexes was found to be 1:1 (drug: reagent) for all methods, as deduced by Job's method of continuous variation. Conclusion: The proposed methods were successfully applied for the determination of asenapine maleate in pharmaceutical formulations with good accuracy and precision. Statistical comparison of the results was performed using Student's t-test and variance ratio F-test at the 95% confidence level and there was no significant difference between the reported and proposed methods regarding accuracy and precision. Further, the validity of the proposed methods was confirmed by recovery studies via standard addition technique in accordance with ICH guidelines.

Development and Validation of UV-Spectrophotometric Methods for the Determination of Berberine in Polymeric Nanoparticles

2019 ◽  
Vol 11 (12) ◽  
pp. 1273-1278
Author(s):  
Md Ali Mujtaba
Keyword(s):  
Phosphate Buffer ◽  
Limit Of Detection ◽  
Polymeric Nanoparticles ◽  
Uv Spectroscopy ◽  
Pharmaceutical Formulation ◽  
Limit Of Quantification ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Development And Validation

A simple, specific, economic, accurate, and reproducible UV-spectrophotometric methods were developed and validated for the estimation of berberine (BRC) in bulk and pharmaceutical formulation. The λmax of BRC in 0.1 N hydrochloric acid (pH 1.2), phosphate buffer (pH 6.8), and water was found to be 346 nm, 343 nm and 260 nm respectively. Beer's law was obeyed in the concentration range of 5–30 μg/ml (R2 = 0.9698) in water, 5–25 μg/ml (R2 = 0.9991) in 0.1 N HCl buffer (pH 1.2) and 5–35 μg/ml (R2 = 0.9935) in phosphate buffer (pH 6.8). These methods were tested, and validated for various parameters such as linearity, precision, accuracy, specificity, limit of detection (LOD), and limit of quantification (LOQ) according to ICH guidelines. The method showed good reproducibility and recovery with percent relative standard deviation less than 2%. Moreover, the accuracy and precision obtained implied that UV spectroscopy can be a cheap, reliable, and less time consuming alternative for chromatographic analysis. The proposed methods were successfully applied for the determination of BRC in pharmaceutical formulation. The BRC estimated from the formulation was found to be well within limits (±5% of the labelled content of the formulations). The proposed methods are highly sensitive, precise, accurate, and can be employed for the routine analysis of berberine in bulks as well as in the commercial formulations.

scholarly journals A simple spectrophotometric method for the determination of captopril in pharmaceutical preparations using ammonium molybdate

2010 ◽  
Vol 35 (3) ◽  
pp. 179-188 ◽  
Author(s):  
P. R. S Ribeiro ◽  
L Pezza ◽  
H. R Pezza
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Reduction Reaction ◽  
Ammonium Molybdate ◽  
Excellent Correlation ◽  
Limit Of Quantification ◽  
The Common

A simple, rapid and sensitive spectrophotometric method for the determination of captopril (CPT) in pharmaceutical formulations is proposed. This method is based on the reduction reaction of ammonium molybdate, in the presence of sulphuric acid, for the group thiol of CPT, producing a green compound (λ max 407 nm). Beer's law is obeyed in a concentration range of 4.60 x 10-4 - 1.84 x 10-3 mol l-1 of CPT with an excellent correlation coefficient (r = 0.9995). The limit of detection and limit of quantification were 7.31 x 10-6 e 2.43 x 10-5 mol l-1 of CPT, respectively. The proposed method was successfully applied to the determination of CPT in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in the formulations. The results obtained by the proposed method were favorably compared with those given by the official reported method at 95 % confidence level.

scholarly journals A SIMPLE SPECTROPHOTOMETRIC METHOD FOR THE DETERMINATION OF CAPTOPRIL IN PHARMACEUTICAL PREPARATIONS USING AMMONIUM MOLYBDATE

2018 ◽  
Vol 35 (3) ◽  
pp. 179
Author(s):  
Paulo Roberto Da Silva Ribeiro ◽  
Leonardo Pezza ◽  
Helena Redigolo Pezza
Keyword(s):  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Pharmaceutical Formulations ◽  
Reduction Reaction ◽  
Ammonium Molybdate ◽  
Excellent Correlation ◽  
Limit Of Quantification ◽  
The Common

A simple, rapid and sensitive spectrophotometric method for the determination of captopril (CPT) in pharmaceutical formulations is proposed. This method is based on the reduction reaction of ammonium molybdate, in the presence of sulphuric acid, for the group thiol of CPT, producing a green compound (λmax 407 nm). Beer’s law is obeyed in a concentration range of 4.60 x 10-4 – 1.84 x 10-3 mol l-1 of CPT with an excellent correlation coefficient (r = 0.9995). The limit of detection and limit of quantification were 7.31 x 10-6 e 2.43 x 10-5 mol l-1 of CPT, respectively. The proposed method was successfully applied to the determinationof CPT in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in the formulations. The results obtained by the proposed method were favorably compared with those given by the official reported method at 95 % confidence level.

Sign in / Sign up

Export Citation Format

Share Document