scholarly journals A Simple and Rapid Spectrophotometric Method for Nitrite Detection in Small Sample Volumes

Chemosensors ◽  
2021 ◽  
Vol 9 (7) ◽  
pp. 161
Author(s):  
Yudtapum Thipwimonmas ◽  
Janjira Jaidam ◽  
Kritsada Samoson ◽  
Vacharachai Khunseeraksa ◽  
Apichai Phonchai ◽  
...  

A simple, rapid, and environmentally-friendly spectrophotometric method for nitrite detection was developed. Detection was based on a redox reaction with iodide ions in an acidic condition. The reaction was evaluated by detecting the increase in absorbance of the colored product of iodine at 362 nm wavelength. To obtain a good spectrophotometric performance, the iodide ions concentration, hydrochloric acid concentration, and reaction time were optimized. In the optimal condition, the developed spectrophotometric method provided a linear range of 0.0625 to 4.00 mg L−1 (r = 0.9985), reaction time for 10 min, a limit of detection of 25 µg L−1, and a limit of quantitation of 85 µg L−1. This method showed good repeatability (RSD < 9.21%), high sample throughput (9 samples min−1), and good accuracy (recovery = 88 ± 2 to 99.5 ± 0.4%). The method has the potential to be used in crime scene investigations as a rapid screening test for gunshot residue detection via nitrite detection.

2021 ◽  
Vol 10 (1) ◽  
pp. 22-25
Author(s):  
Firake Bhushan M. ◽  
Pathak Pranjalee V. ◽  
Dorik Pallavi K. ◽  
Siddaiah M.

UV spectrophotometry is an analytical technique used routinely for qualitative and quantitative assay due the low cost and reliability during analysis. An simple, efficient, rapid, sensitive, precise and economical UV Spectrophotometric method has been developed for estimation of agomelatine from bulk and pharmaceutical formulation. The method was developed and validated according to International Conference on Harmonization (ICH Q2 R1) guidelines.  The λmax of agomelatine in acetonitrile was found to be 229.6 nm. The analytical method validation parameters linearity, precision, accuracy, robustness were studied according to International Conference on Harmonization guidelines. Pure drug concentration was prepared in the range of 1-10 μg/ml and the linear regression analysis data showed good linear relationship with correlation coefficient value 0.9937. The precision of the method was studied as an intra- day, inter-day variations with value less than 2 % RSD. The limit of detection and limit of quantitation were found to be 0.577 and 1.248 μg/ml, respectively. Recoveries were found to be in the range of 100.815 to 101.744 % and % RSD was less than 2 %. This proposed UV spectroscopic method is simple and suitable for routine analysis. Keywords: Keywords: Agomelatine, Validation, UV Spectrophotometric method


Author(s):  
Jaspreet Kaur ◽  
Daljit Kaur ◽  
Sukhmeet Singh

Objective: A simple, accurate, and selective ultraviolet-spectrophotometric method has been developed for the estimation of febuxostat in the bulk and pharmaceutical dosage forms.Method: The method was developed and validated according to International Conference on Harmonization (ICH Q2 R1) guidelines. The developed method was validated statistically with respect to linearity, range, precision, accuracy, ruggedness, limit of detection (LOD), limit of quantitation (LOQ), and recovery. Specificity of the method was demonstrated by applying different stressed conditions to drug samples such as acid hydrolysis, alkaline hydrolysis, oxidative, photolytic, and thermal degradation.Results: The study was conducted using phosphate buffer pH 6.8 and λmax was found to be 312 nm. Standard plot having a concentration range of 1–10 μg/ml showed a good linear relationship with R2=0.999. The LOD and LOQ were found to be 0.118 μg/ml and 0.595 μg/ml, respectively. Recovery and percentage relative standard deviations were found to be 100.157±0.332% and <2%, respectively.Conclusion: Proposed method was successfully applicable to the pharmaceutical formulations containing febuxostat. Thus, the developed method is found to be simple, sensitive, accurate, precise, reproducible, and economical for the determination of febuxostat in pharmaceutical dosage forms.


2012 ◽  
Vol 9 (2) ◽  
pp. 993-998
Author(s):  
Madhusudhanareddy Induri ◽  
Bhagavan Raju M. ◽  
Rajendra Prasad Y. ◽  
Pavankumar Reddy K.

The objective of present study was to develop and validate an analytical method for quantitative determination and dissolution studies of glimepiride in tablets. The glimepiride shows absorption maxima at 225 nm and obeyed Beer's law in the range of 6.0 – 14.0 µg/mL. The limit of detection and limit of quantitation were 0.06, and 0.17 µg/mL respectively. Percentage recovery of glimepiride for the proposed method ranged from 99.32 to 100.98% indicating no interference of the tablet excipients. It was concluded that the proposed method is simple, easy to apply, economical and used as an alternative to the existing spectrophotometric and non-spectrophotometric methods for the routine analysis of glimepiride in pharmaceutical formulations andin vitrodissolution studies.


Author(s):  
Chandani Makvana ◽  
Satyajit Sahoo

A simple, rapid, precise, accurate and sensitive spectrophotometric method has been developed for the simultaneous estimation and validation of Nebivolol Hydrochloride (NEB) and Valsartan (VAL) in pure and combined tablet dosage forms. Pure drug samples of NEB and VAL were dissolved in 67 mM Phosphate buffer pH 6.8 with 0.5% sodium dodecyl sulphate (SDS) and found to have absorbance maxima at 280 nm for NEB and 250 nm for VAL, respectively. The linearity lies between 10-70μg/ml for NEB and 10-60μg/ml for VAL in this method. The correlation coefficient (r2) was found to be 0.9965 for NEB and 0.9960 for VAL. The % recoveries obtained were 95.65%-109.85% for NEB and 97.42%-101.43% for VAL. The % RSD found 0.271%-1.490% for intraday and 0.334%-1.917% for interday for NEB and 0.188%-0.944% for intraday and 0.392%-1.197% for interday for VAL. The limit of detection and limit of quantitation for NEB were found to be 4.608μg/ml and 13.965μg/ml respectively and the limit of detection and limit of quantitation for VAL were found to be 4.348μg/ml and 13.178μg/ml respectively. Simultaneous calibration of both drugs in 67 mM Phosphate buffer pH 6.8 with 0.5% SDS shows that λmax of one drug does not interfere on the λmax of other drug. Recovery study was performed to confirm the accuracy of the method. The results of analysis have been validated statistically by recovery studies as per International Conference on Harmonization guidelines. The method showed good reproducibility and recovery with % RSD Lessthan 2. Hence, this proposed method was found to be rapid, specific, precise and accurate and can be successfully applied for the routine analysis of NEB and VAL in pure and combined tablet dosage form.


2019 ◽  
Vol 65 (2) ◽  
pp. 55-59 ◽  
Author(s):  
Béla Kovács ◽  
Réka Molnár ◽  
Előd Ernő Nagy ◽  
Éva Katalin Kelemen ◽  
Blanka Székely-Szentmiklósi ◽  
...  

AbstractObjective: The present work offers a fast, reliable and easy UV spectrophotometric method for the assay of strontium ranelate from bulk samples and pharmaceutical dosage form.Methods: The proposed method uses 0.1% V/V trichloroacetic acid as dissolution medium for spectrophotometric analysis, by signal detection at 321 nm. The method was validated according to the currently in-force international guidelines for linearity, accuracy, precision, robustness, limit of detection and quantification.Results: The method was found to be linear in the range of 5-100 µg mL-1 (R2 > 0.999). Method accuracy was found in-between 98.87-100.41%, showing good linear correlation as well (R2 = 0.9997). The concentrations for limit of detection and limit of quantitation were found 1.13 µg mL-1 and 3.77 µg mL-1, resp. The proposed method showed good intra- and interday precision, with low RSD values of 0.53-1.24% and 1.11%, resp.Conclusions: Stability studies performed by both HPLC and UV spectrophotometric methods revealed that the active substance is highly susceptible to acidic hydrolysis, oxidation and exposure to high temperature.


2021 ◽  
Vol 21 (1) ◽  
Author(s):  
NERDY NERDY ◽  
EFFENDY DE LUX PUTRA ◽  
NILSYA FEBRIKA ZEBUA ◽  
CHRISTICA ILSANNA SURBAKTI ◽  
JIHAN SAFIRA

Metamizole is a nonsteroidal antiinflammatory drug (NSAID) that functions as an analgesic, antipyretic, and antiinflammatory. Examination of active substance contents is a requirement that must be met to ensure the quality of drug preparations. The aims of this study were to develop and validate the Fourier Transform Infrared spectrophotometric method for the quantitation of metamizole content in marketed tablet preparation. Identification and determination of metamizole contents by Fourier Transform Infrared spectrophotometric method used methanol solvent in the wavenumber range 4000 cm–1 to 650 cm–1. The results showed that the specific wavenumbers of metamizole were 1649.3 cm–1; 1623.3 cm–1; and 1589.7 cm–1; and the contents metamizole in marketed tablet preparation ranged from (97.954 ± 0.121)% to (104.541 ± 0.257)%. From the validation method, the recovery result is 100.129%; the relative standard deviation is 0.057%; the limit of detection is 2.09526 mg/mL; the limit of quantitation is 6.34928 mg/mL; and the range 40 mg/mL to 60 mg/mL. The quantitation of metamizole contents can be carried out by Fourier Transform Infrared spectrophotometric method with accurate and precise quantitation results.


INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (12) ◽  
pp. 31-36
Author(s):  
N Mallikarjuna Rao ◽  
◽  
D. Gowrisankar

A novel stability indicating UV spectrophotometric method for the quantitative determination of cinacalcet hydrochloride, a calcimimetic, in bulk and tablet dosage forms was developed in the present work. The parameters linearity, precision, accuracy, limit of detection and limit of quantitation were studied according to International Conference on Harmonization guidelines. UV spectroscopic determination was carried out at an absorption maximum of 281 nm using methanol as solvent. In the UV spectroscopic method, linearity over the concentration range of cinacalcet hydrochloride was found to be 15-35 μg/mL with a correlation coefficient of 0.9992. Results of the analysis were validated statistically and by recovery studies. Forced degradation studies were conducted under various conditions. The proposed method is simple, rapid, precise and accurate and can be used for the reliable quantitation of cinacalcet hydrochloride in commercial pharmaceutical dosage forms.


2016 ◽  
Vol 24 (2) ◽  
pp. 88-101
Author(s):  
Mohauman Mohammad Al-Rufaie

Abstract A sensitive, simple and rapid spectrophotometric procedure for the assay of trace quantities of sulfadiazine (SDZ) drug as bulk and in diluted solution is characterized. The procedure depends on the diazotization reaction which is produced by coupling SDZ with (4-amino-2-hydroxy acetophenon) (AHA) to produce an intense colored complex spectrophotometrically determined at 410 nm. Beer’s law was applied in the range of concentration 0.5 - 15 ppm; the molar absorptivity and Sandell’s sensitivity were 2.8484 × 104 L mol-1 cm-1 and 0.008 μg cm-2 respectively. The method limit of detection (LOD) was 0.443 μg mL-1 and LOQ (the method limit of quantitation) was 0.249 μg mL-1. The procedure is not based on solvent extraction and the additives and excipients do not significantly influence the developed procedure.


2009 ◽  
Vol 6 (s1) ◽  
pp. S163-S170 ◽  
Author(s):  
R. Singh Gujral ◽  
S. Manirul Haque ◽  
P. Shanker

An accurate and validated spectrophotometric method was developed for the determination of gabapentin. This is simple, sensitive and low cost UV spectrophotometric method. The method is based on the direct measurement of the native absorbance of the drug. The detection was done at 210 nm. The method was linear in the range of 0.25 - 3.5 µ g/mL with correlation coefficient of 0.9999. It is validated according to the ICH guidelines with respect to linearity, selectivity, accuracy and precision, limit of quantitation and limit of detection. The method has been applied to assess gabapentin in pharmaceutical formulations with good accuracy and precision and relatively free of interference from coexisting substances.


2008 ◽  
Vol 91 (1) ◽  
pp. 52-58 ◽  
Author(s):  
Jlia Menegola ◽  
Martin Steppe ◽  
Elfrides E S Schapoval

Abstract Column high-performance liquid chromatographic (LC) and UV spectrophotometric methods for the quantitative determination of citalopram, a potent and selective serotonin reuptake inhibitor, in tablets were developed. The parameters linearity, precision, accuracy, specificity, robustness, limit of detection, and limit of quantitation were studied according to International Conference on Harmonization guidelines. Chromatography was carried out by the reversed-phase technique on an ACE C18 column with a mobile phase composed of 0.30 triethylamine solutionacetonitrile (55 + 45, v/v) adjusted to pH 6.6 with 10 ortho-phosphoric acid at a flow rate of 1.0 mL/min and 25C. The UV spectrophotometric method was performed at 239 nm. The linearity of the LC method was in the range of 10.0070.00 g/mL, and 2.5017.50 g/mL for the UV spectrophotometric method. The interday and intraday assay precision was &lt;1.5 (relative standard deviation) for the LC and UV spectrophotometric methods. The recoveries were in the range 100.70101.35 for the LC method and 98.4898.65 for the UV spectrophotometric method. Statistical analysis by Student's t-test showed no significant difference between the results obtained by the 2 methods. The proposed methods are highly sensitive, precise, and accurate and can be used for the reliable quantitation of citalopram in tablets.


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