scholarly journals GAS CHROMATOGRAPHIC DETERMINATION OF 23 ORGANOPHOSPHORUS PESTICIDES RESIDUE IN BOTTLE GUARD MATRIX

2018 ◽  
Vol 10 (1) ◽  
pp. 53
Author(s):  
Sudeep Mishra ◽  
Lalitesh Kr. Thakur ◽  
Neelam Richhariya
Keyword(s):  
Limit Of Detection ◽  
Organophosphorus Pesticides ◽  
Chromatographic Determination ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Residue Levels ◽  
The Mean ◽  
Pesticides Residue ◽  
Chromatographic Mass

Objective: To validate in-house QuEChERS method, which scrutinizes and quantify the residue levels of some most frequently used organophosphorus pesticides and to prove a complete workflow for routine multi-residue pesticide analysis in representative bottle guard matrices and study the persistence of 23 organ phosphorus pesticides.Methods: QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction method was followed. Method validation and residue screening of bottle guard samples were conducted by GC-FPD (Gas Chromatography-Flame Photometric Detector) were used to analyse the presence of pesticides whereas confirmation of pesticides was done by GC-MS (Gas Chromatographic-Mass Spectrometer). Results: For bottle guard matrix, LOD (limit of detection) and LOQ (limit of quantification) values are lowest for phorate (0.005 mg/kg and 0.015 mg/kg) and highest for parathion-methyl (0.1 mg/kg and 0.3 mg/kg) respectively. Calibration curve, was plotted between an area of 23 pesticide standard mixture against seven different concentration levels of 0.01, 0.02, 0.05, 0.10, 0.20, 0.50, 1.00 mg/kg with regression coefficient (R2) are in the range of 0.978-0.994. The mean recovered amount at 0.05 mg/kg spikeing concentration are in the range of lowest 0.0413 mg/kg to highest 0.0467 mg/kg and relative standard deviation are in the range of lowest 2.2 to highest 8.571.Conclusion: For ensuring exposure to contaminants, especially by dietary intake, Robust analytical methods were validated for carrying out both research and monitoring programmes and thus for defining limitations and supporting enforcement of regulations.

scholarly journals A novel LC-MS method development and validation for the determination of phenyl vinyl sulfone in eletriptan hydrobromide

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Indhu Priya Mabbu ◽  
G. Sumathi ◽  
N. Devanna
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Vinyl Sulfone ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Pressure Chemical Ionization ◽  
Pressure Chemical ◽  
Development And Validation ◽  
Phenyl Vinyl

Abstract Background The aim of the present method is to develop and validate a specific, sensitive, precise, and accurate liquid chromatography-mass spectrometry (LC-MS) method for the estimation of the phenyl vinyl sulfone in the eletriptan hydrobromide. The effective separation of the phenyl vinyl sulfone was achieved by the Symmetry C18 (50 × 4.6 mm, 3.5 μm) column and a mobile phase composition of 0.1%v/v ammonia buffer to methanol (5:95 v/v), using 0.45 ml/min flow rate and 20 μl of injection volume, with methanol used as diluent. The phenyl vinyl sulfone was monitored on atomic pressure chemical ionization mode mass spectrometer with positive polarity mode. Results The retention time of phenyl vinyl sulfone was found at 2.13 min. The limit of detection (LOD) and limit of quantification (LOQ) were observed at 1.43 ppm and 4.77 ppm concentration respectively; the linear range was found in the concentration ranges from 4.77 to 27.00 ppm with regression coefficient of 0.9990 and accuracy in the range of 97.50–102.10%. The percentage relative standard deviation (% RSD) for six replicates said to be injections were less than 10%. Conclusion The proposed method was validated successfully as per ICH guidelines. Hence, this is employed for the determination of phenyl vinyl sulfone in the eletriptan hydrobromide.

scholarly journals Determination of 77 Multiclass Pesticides and Their Metabolitesin Capsicum and Tomato Using GC-MS/MS and LC-MS/MS

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Graphitized Carbon Black ◽  
Limit Of Quantification ◽  
Gas And Liquid Chromatography ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Primary Secondary Amine

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.

scholarly journals Determination of uric acid in human serum by an enzymatic method using N-methyl-N-(4-aminophenyl)-3-methoxyaniline reagent

2003 ◽  
Vol 68 (8-9) ◽  
pp. 691-698 ◽  
Author(s):  
Milena Jelikic-Stankov ◽  
Predrag Djurdjevic ◽  
Dejan Stankov
Keyword(s):  
Uric Acid ◽  
Human Serum ◽  
Limit Of Detection ◽  
Ascorbate Oxidase ◽  
Acid Oxidation ◽  
Uric Acid Concentration ◽  
Enzymatic Method ◽  
Limit Of Quantification ◽  
Relative Standard

In this work a new enzymatic method for the determination of uric acid in human serum has been developed. The method is based on the oxidative coupling reaction between the N-methyl-N-(4-aminophenyl)-3-methoxyaniline (NCP) reagent and the hydrogen ? donor reagent N-ethyl-N-(2-hydroxy-3-sulfopropyl)-3-methylaniline (TOOS), in the system involving three enzymes: uricase, peroxidase and ascorbate oxidase. Using this method uric acid could be determined in concentrations up to 1.428 mmol/L, with a relative standard deviation of up to 1.8 %. The effect of the medium pH and the NCP concentration on the linearity of the chromogen absorbance versus the uric acid concentration curve was investigated. The influence of the uricase activity on the maximum rate of uric acid oxidation was also examined. The use of the NCP reagent demonstrated a more precise and more sensitive determination of the uric acid compared to the determination with 4-aminoantipyrine (4-AA) as the coupling regent. The sensitivity of the method determined from the calibration curve was 0.71 absorbance units per mmol/L of uric acid; the limit of detection was LOD = 0.0035 mmol/L and the limit of quantification was LOQ = 0.015 mmol/L of uric acid.

scholarly journals Spectrophotometric determination of Phenylephrine hydrochloride and Salbutamol sulphate drugs in pharmaceutical preparations using diazotized Metoclopramide hydrochloride

2015 ◽  
Vol 12 (1) ◽  
pp. 167-177 ◽  
Author(s):  
Baghdad Science Journal
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Correlation Coefficients ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Salbutamol Sulphate ◽  
Phenylephrine Hydrochloride ◽  
Relative Standard ◽  
Metoclopramide Hydrochloride

A spectrophotometric method has been proposed for the determination of two drugs containing phenol group [phenylephrine hydrochloride (PHP) and salbutamol sulphate (SLB)] in pharmaceutical dosage forms. The method is based on the diazotization reaction of metoclopramide hydrochloride (MCP) and coupling of the diazotized reagent with drugs in alkaline medium to give intense orange colored product (?max at 470 nm for each of PHP and SLB). Variable parameters such as temperature, reaction time and concentration of the reactants have been analyzed and optimized. Under the proposed optimum condition, Beer’s law was obeyed in the concentration range of 1-32 and 1-14 ?g mL-1 for PHP and SLB, respectively. The limit of detection (LOD) and limit of quantification (LOQ) for each of PHP and SLB were 0.60, 0.52 ?g mL-1 and 2.02, 1.72 ?g mL-1, respectively. No interference was observed from common excipients present in pharmaceutical preparations. The good correlation coefficients and low relative standard deviation assert the applicability of this method. The suggested method was further applied for the determinations of drugs in commercial pharmaceutical preparations, which was compared statistically with reference methods by means of t- test and F- test and were found not to differ significantly at 95% confidence level. The procedure was characterized by its simplicity with accuracy and precision.

scholarly journals Validated TLC-densitometry method for determination of cetirizine dihydrochloride in tablet dosage form

2013 ◽  
Vol 3 (1) ◽  
pp. 208-210
Author(s):  
Nia Kristiningrum ◽  
Ellsy Novita Martyanti
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Pharmaceutical Journal ◽  
Limit Of Quantification ◽  
Quality Control Testing ◽  
Relative Standard ◽  
Tablet Formulations ◽  
Tablet Dosage ◽  
Chloroform Methanol

A rapid, reproducible and accurate TLC method was developed for the determination of Cetirizine Dihydrochloride in tablet. The analytes were dissolved with ethanol 70% and chromatographed on silica Gel GF 254 TLC plate using chloroform : methanol : ethyl acetate in the ratio of 2 : 7 : 3 (v/v) as mobile phase. Quantitative analysis was done through densitometric measurement at wavelength 234 nm. Method was found linear over the concentration range of 400 – 1600 ng/spot with the correlation coefficient of 0.996. Specificity showed calculation of purity and identity more than 0.99. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were 75.54 and 226.64 ng/spot. The relative standard deviation of this method was 0.86% whereas the means of the recovery data was 100.54 ± 0.11%. The proposed method has been applied to the determination of Cetirizine Dihydrochloride in commercial tablet formulations and the result were 96.97 ± 0.86 % for brand A and 100.57 ± 1.17 % for brand B. The developed method was successfully used for the assay of Cetirizine Dihydrochloride. This method is simple, sensitive and precise; it can be used for the routine quality control testing of marketed formulations.DOI: http://dx.doi.org/10.3329/icpj.v3i1.17294 International Current Pharmaceutical Journal, December 2013, 3(1): 208-210

scholarly journals Micellar Liquid Chromatographic Determination of Carbaryl and 1-Naphthol in Water, Soil, and Vegetables

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Mei-Liang Chin-Chen ◽  
Maria Rambla-Alegre ◽  
Abhilasha Durgbanshi ◽  
Devasish Bose ◽  
Sandeep K. Mourya ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Cetylpyridinium Chloride ◽  
Sodium Dodecyl ◽  
Chromatographic Determination ◽  
Limit Of Quantification ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

A liquid chromatographic procedure has been developed for the determination of carbaryl, a phenyl-N-methylcarbamate, and its main metabolite 1-naphthol, using a C18 column (250’mm’ × ’4.6’mm) with a micellar mobile phase and fluorescence detection at maximum excitation/emission wavelengths of 225/333’nm, respectively. In the optimization step, surfactants sodium dodecyl sulphate (SDS), Brij-35 andN-cetylpyridinium chloride monohydrate, and organic solvents propanol, butanol, and pentanol were considered. The selected mobile phase was 0.15’M SDS-6% (v/v)-pentanol-0.01’M NaH2PO4buffered at pH 3. Validation studies, according to the ICH Tripartite Guideline, included linearity (r>0.999), limit of detection (5 and 18’ng mL-1, for carbaryl and 1-naphthol, resp.), and limit of quantification (15 and 50’ng mL-1, for carbaryl and 1-naphthol, resp.), with intra- and interday precisions below 1%, and robustness parameters below 3%. The results show that the procedure was adequate for the routine analysis of these two compounds in water, soil, and vegetables samples.

Liquid Chromatographic Determination of Fluometuron and Metabolites in Soil

1991 ◽  
Vol 74 (4) ◽  
pp. 671-673 ◽  
Author(s):  
Thomas C Mueller ◽  
Thomas B Moorman
Keyword(s):  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Silt Loam ◽  
Soil Extracts ◽  
Liquid Chromatographic Separation ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Soluble Components

Abstract A rapid, sensitive method Is described for the determination of fluometuron and Its soil metabolites In 4 soil types. The method consists of extraction of moist soil samples with methanol, filtration, liquid chromatographic separation of methanol-soluble components using a C18 column, and fluorescence detection with excitation at 292 nm and emission measured at 345 nm. Fluometuron recoveries from fortified soils were >90% from the Dundee, Okalona, Cecil, and Ships soils. Recoveries from a Dundee silt loam for desmethyl fluometuron, 3-(trlfluoromethyl)phenyl urea, and 3- (trifluoromethyl)anillne were 77, 77, and 35%, respectively. Average percent relative standard deviations of Dundee soil extracts were 5.3% for fluometuron and <8.0% for each metabolite. The limit of detection for fluometuron and each of its soil metabolites was 25 ng/g soil.

High Performance Liquid Chromatographic Determination of Phenothiazine Residues in Sheep Tissues

1980 ◽  
Vol 63 (5) ◽  
pp. 988-991
Author(s):  
Graeme L Blackman ◽  
Ah Chai Ho ◽  
Alex Jozsa ◽  
John D Kelly
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Tissue Samples ◽  
Silica Column ◽  
Liquid Chromatographic Determination ◽  
Residue Levels ◽  
Liquid Chromatographic

Abstract A high performance liquid chromatographic (HPLC) technique is described for the determination of residue levels of the anthelmintic drug phenothiazine in sheep tissues. Phenothiazine was administered to sheep which were slaughtered after withholding periods of 24, 48, and 72 h. Residues of phenothiazine were then extracted from tissue samples by homogenization in methanol. The HPLC analysis of the extracts involved separation on a 10 μm silica column using a mobile phase of 0.3% n-propanol in cyclohexane. The lower limit of detection by ultraviolet absorption at 254 nm was 0.05 ppm

scholarly journals Ultraviolet Spectrophotometric Method for Determination of Glipizide in Presence of Liposomal/Proliposomal Turbidity

2013 ◽  
Vol 2013 ◽  
pp. 1-5
Author(s):  
Neelkant Prasad ◽  
Roshan Issarani ◽  
Badri Prakash Nagori
Keyword(s):  
Spectrophotometric Method ◽  
Calibration Curve ◽  
Limit Of Detection ◽  
Quantitative Estimation ◽  
Uv Detection ◽  
Limit Of Quantification ◽  
Relative Standard ◽  
Precision And Accuracy ◽  
Clear Solution

A simple and sensitive ultraviolet spectrophotometric method for quantitative estimation of glipizide in presence of lipid turbidity is described to avoid false estimation due to diffraction by turbidity. UV detection was performed at 230 nm, 225 nm, and 235 nm, and the calibration curve was plotted between resultant of absorbance of [230 nm − (225 nm + 235 nm)/2] and concentration of analyte. The calibration curve was linear over the concentration range tested (1–20 μg/mL) with limit of detection of 0.27 μg/mL and limit of quantification of 0.82 μg/mL. Percent relative standard deviations and percent relative mean error, representing precision and accuracy, respectively, for clear as well as turbid solutions, were found to be within acceptable limits, that is, always less than 0.69 and 0.41, respectively, for clear solution and 0.65 and 0.47, respectively, for turbid solution. Conclusively, our method was successfully applied for the determination of glipizide in clear as well as turbid solutions, and it was found that the drug analyte in both types of solutions can be detected from the same calibration curve accurately and precisely and glipizide entrapped in the liposomes or in proliposomal matrix was not detected.

scholarly journals Occurrence of aflatoxins in peanuts and peanut products determined by liquid chromatography with fluorescence detection

2013 ◽  
pp. 27-35 ◽  
Author(s):  
Biljana Stojanovska-Dimzoska ◽  
Zehra Hajrulai-Musliu ◽  
Elizabeta Dimitrieska-Stojkovic ◽  
Risto Uzunov ◽  
Pavle Sekulovski
Keyword(s):  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
Limit Of Detection ◽  
Total Content ◽  
Immunoaffinity Column ◽  
Limit Of Quantification ◽  
Three Samples ◽  
The Mean ◽  
Positive Results

Liquid chromatography with fluorescence detection using immunoaffinity column clean-up was a method described for determination of aflatoxins (AFB1, AFB2, AFG1 and AFG2) in peanuts and peanut based products. The validation of the procedure was performed. Good coefficient of correlation was found for all aflatoxins in the range of 0.9993-0.9999. Limit of detection (LOD) and limit of quantification (LOQ) ranged from 0.003-0.005 mg/kg and 0.009-0.023 mg/kg, respectively, which was acceptable. The mean recovery for total aflatoxins was 88.21%. The method also showed acceptable precision values in the range of 0.171-2.626% at proposed concentration levels for all four aflatoxins. RSDR values (within laboratory reproducibility) calculated from the results showed good correlation between two analysts for all aflatoxins and they ranged from 4.93-11.87%. The developed method was applied for the determination of aflatoxins in 27 samples of peanuts and peanut based products. The results showed that 21 peanut samples (77.7%) were below LOD of the method. Three samples had positive results over the MRL. There was one extreme value recorded for the total aflatoxins in peanut (289.2 mg/kg) and two peanut based products, peanut snack and peanut, with total content of aflatoxins being 16.3 mg/kg and 8.0 mg/kg, respectively. The obtained results demonstrated that the procedure was suitable for the de?termination of aflatoxins in peanuts and peanut based products and it could be implemented for the routine analysis.

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