scholarly journals Development of a simple HPLC procedure for the determination of prochloraz residues in mushrooms

2021 ◽  
Author(s):  
Csaba Csutoras ◽  
Andras Misz ◽  
Csaba Nagy-Koteles ◽  
Nora Bakos-Barczi ◽  
Laszlo Racz
Keyword(s):  
Preparation Method ◽  
Limit Of Detection ◽  
Sample Preparation Method ◽  
Limit Of Quantification ◽  
Simple Method ◽  
Mushroom Production ◽  
Modified Quechers ◽  
Cost Efficient ◽  
Solid Liquid

AbstractA simple HPLC-UV procedure is described in our paper which is suitable for the rapid and cost-efficient determination of prochloraz in mushrooms. Prochloraz is the only fungicide in EU which use is allowed in mushroom production. The aim of our work was the development of a simple method that is suitable for the control of this pesticide in everyday analyses during mushroom production. The procedure involves a simple sample preparation method based on solid-liquid extraction (modified QuEChERS extraction method EN 15662) followed by an HPLC-UV determination (recovery: 97–99%; limit of detection LOD: 0.01 mg/kg; limit of quantification LOQ: 0.05 mg/kg).

Determination of multiple organochlorine pesticide residues in shrimp using modified QuEChERS extraction and gas chromatography

2018 ◽  
Vol 16 (1) ◽  
pp. 81-93
Author(s):  
MDH Prodhan ◽  
SN Alam
Keyword(s):  
Gas Chromatography ◽  
Organochlorine Pesticide ◽  
Pesticide Residues ◽  
Limit Of Detection ◽  
Residue Analysis ◽  
Limit Of Quantification ◽  
Modified Quechers ◽  
Endosulfan Sulphate ◽  
Organochlorine Pesticide Residues

Determination of organochlorine pesticide residues in shrimp is very important to ensure the consumer’s safety and to fulfill the importer’s demand. Therefore, a simple and efficient multiple organochlorine pesticide residues analytical method using quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction technique and Gas Chromatography coupled with Electron Capture Detector (ECD) has been developed and validated for the determination of 19 organochlorine pesticides (α- BHC, δ- BHC, β- BHC, γ- BHC, Heptachlor, Aldrin, Heptachlor Epoxide, γ- Chlordane, α- Chlordane, α- Endosulfan, 4,4 DDE, Dieldrin, Endrin, 4,4 DDD, β- Endosulfan, 4,4 DDT, Endosulfan sulphate, Methoxychlor, and Endrin Ketone) in shrimp. The method was validated by evaluating the accuracy, precision, linearity, limit of detection (LOD) and limit of quantification (LOQ). The average recoveries of the selected pesticides ranged from 84% to 106% with RSDr ≤ 14% in four fortification levels of 0.05, 0.1, 0.2 and 0.3 mg kg-1. The linearity was ≥ 0.996 for all of the selected pesticides with matrix matched calibration standards. The LOD ranged from 0.003 to 0.009 mg kg-1 and the LOQ was 0.05 mg kg-1. This method was applied successfully for the residue analysis of 40 shrimp samples collected from different regions in Bangladesh.SAARC J. Agri., 16(1): 81-93 (2018)

Gas Chromatographic Determination of p-Chloroaniline in a Chlorhexidine Digluconate-Containing Alcohol Foam Surgical Scrub Product

1994 ◽  
Vol 77 (3) ◽  
pp. 583-586 ◽  
Author(s):  
Walter K Gavlick ◽  
Paula K Davis
Keyword(s):  
Dynamic Range ◽  
Preparation Method ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Chlorhexidine Digluconate ◽  
Linear Dynamic Range ◽  
Sample Preparation Method ◽  
Flame Ionization ◽  
Limit Of Quantitation

Abstract A gas chromatographic (GC) method with flame ionization detection was developed to separate and quantitate p-chloroaniline (PCA) from other components in a chlorhexidine digluconate (CHG)-containing alcohol foam surgical scrub product. A simple sample preparation method was developed in which 1-butanol was used to dissolve the foam and precipitate the CHG, which otherwise would interfere with the GC analysis. The method was validated with respect to linear dynamic range, precision, accuracy, selectivity, limit of detection, and limit of quantitation.

scholarly journals Pesticide Residues Recovery studies by QuEChERS Sample Technique Using Gas Chromatography

2017 ◽  
Vol 104 (.1-.4) ◽  
Author(s):  
Sivanandha Reddy C ◽  
◽  
Subba Reddy G V
Keyword(s):  
Gas Chromatography ◽  
Sunflower Oil ◽  
Pesticide Residues ◽  
Preparation Method ◽  
Limit Of Detection ◽  
Sample Preparation Method ◽  
Limit Of Quantification ◽  
Target Analytes ◽  
Sample Technique ◽  
Standard Solution

The modified Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) sample preparation method was developed and validated for quantification of trace level of dicofol, chlordane and dieldrin pesticides in sunflower oil. The proposed method was applied for extraction of pesticides in sunflower oil and results were plotted with the help of matrix-matched calibration using relative responses versus standard solution. The quantification of pesticide residues carried out in sunflower oil by Gas Chromatography coupled with ECD detector. The method reveals that experimental results were satisfactory in respect of various analytical parameters such as linearity, recovery and precision. The limit of detection (LOD) and limit of quantification (LOQ) for target analytes were in the range of 0.001–0.011 mgkg-1 and 0.002–0.030 mgkg-1 respectively. The influence activated charcoal addition to the sorbents for the recovery of target analyte was also studied and presented in the results.

scholarly journals Development and Validation of an Analytical Method for Determination of Ergot Alkaloids in Animal Feedingstuffs with High Performance Liquid Chromatography-fluorescence Detection

2016 ◽  
Vol 19 (3) ◽  
pp. 559-565 ◽  
Author(s):  
E. Kowalczyk ◽  
E. Patyra ◽  
A. Grelik ◽  
K. Kwiatek
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Fluorescence Detection ◽  
High Performance ◽  
Limit Of Detection ◽  
Ergot Alkaloids ◽  
Coefficient Of Determination ◽  
Limit Of Quantification ◽  
Modified Quechers

Abstract A high performance liquid chromatography combined with fluorescence detection (HPLC-FLD) method was developed for determination of five ergot alkaloids (EA): ergometrine, ergotamine, ergocornine, ergocrypine and ergocristine in animal feedingstuffs. The method was based on the application of QuEChERS salts for extraction and modified QuEChERS dispersive SPE for the cleanup step. Alkaloids separation was performed on a C18, 250 mm x 4.6 mm, 5 μm column with the mobile phase containing ammonium carbonate and acetonitrile. The excitation and emission wavelengths were 330 and 420 nm respectively. The method was validated according to the Commission Decision 2002/657/EC and all parameters are in agreement with the requirements of the Decision. Linearity was determined for the concentration range of 25-400 μg/kg. The coefficient of determination (R2) for all curves was from 0.985 to 0.996. The limit of detection (LOD) was in the range 3.23 to 6.53 μg/kg and the limit of quantification (LOQ) from 11.78 to 13.06 μg/kg. The decision limit (CCα) ranged from 29.56 to 43.08 μg/kg and detection capability (CCβ) from 40.65 to 51.01 μg/kg. The highest coefficient of variation (CV) for repeatability was 14.3% and for reproducibility 15.4%.

scholarly journals A Simple Method for the Screening and Measurement of Phenols in Dendrobium chrysotoxum by a Miniature Mass Detector Using a Matrix Solid-Phase Dispersion Method

2019 ◽  
Vol 2019 ◽  
pp. 1-9 ◽  
Author(s):  
Hongcheng Liu ◽  
Duo Mu ◽  
Tao Lin ◽  
Qiwan Li
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Limit Of Quantification ◽  
Simple Method ◽  
Mass Detector ◽  
Full Scan ◽  
Standard Solution ◽  
New Compounds

The present study aims at building a miniature mass method for the simultaneous determination of 12 phenols including the subtypes of bibenzyl, phenanthrene, and fluorenone, which was used to evaluate the quality of Dendrobium chrysotoxum. Through the full scan mode, new compounds were elucidated. The new compounds were quantified by carrying out the analysis of the ratio of the standard solution areas to new compound areas versus analyte concentration. The limit of detection (LOD) and limit of quantification (LOQ) for phenols were 0.5 µg/mL–1 µg/mL and 1 µg/mL–2 µg/mL, respectively. Average recoveries of phenols were ranged from 83.2% to 97.5%. Reproducibility represented by the RSD percentage was from 2.3% to 8.7%. The average content of the four analytes, erianin, chrysotobibenzyl, confusarin, and moscatilin, were more than 200 mg/kg, and the content of bibenzyl compounds was found to be the highest in Dendrobium chrysotoxum. Among these bibenzyl compounds, erianin was determined as the typical chemical marker from Dendrobium chrysotoxum. The newly established UPLC with a miniature mass detector method was found to be an appropriate tool for the quality assessment of Dendrobium chrysotoxum.

Spectrophotometeric Determination of Trifluoperazine HCL in Pure Forms and Pharmaceutical Preperations

2017 ◽  
Vol 9 (5) ◽  
Author(s):  
Mohammad Hamzah Hamzah ◽  
Rawa M M Taqi ◽  
Muna M. Hasan ◽  
Raid J. M. Al-Timimi
Keyword(s):  
Standard Method ◽  
Limit Of Detection ◽  
Molar Absorptivity ◽  
Dosage Forms ◽  
Oxidizing Agent ◽  
Optimum Conditions ◽  
Limit Of Quantification ◽  
Cerium Ion ◽  
Blank Solution

A simple and accurate spectrophotometric method for the determination of Trifluoperazine HCl in pure and dosage forms was developed. The method is based on the reaction between Trifluoperazine HCl and p-chloroaniline in the presence of cerium ion as oxidizing agent which lead to the formation of violate color product that absorbed at a maximum wavelength 570nm while the blank solution was pink. Under the optimum conditions a linear relationship between the intensity and concentration of TRF in the range 4-50μg/ml was obtained . The molar absorptivity 3.74×103 L.mol-1.cm-1 , Limit of detection (2.21μg/ml), while limit of quantification was 7.39μg/ml. The proposed analytical method was compared with standard method using t-test and F-test , the obtained results shows there is no significant differences between proposed method and standard method. Based on that the proposed method can be used as an alternative method for the determination of TRF in pure and dosage forms.

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 10-GINGEROL IN INDIAN GINGER BY VALIDATED HPTLC METHOD OF SAMPLES COLLECTED ACROSS SUBCONTINENT OF INDIA

2016 ◽  
Vol 8 (12) ◽  
pp. 190
Author(s):  
Kamran Ashraf ◽  
Syed Adnan Ali Shah ◽  
Mohd Mujeeb
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Aluminum Plates ◽  
Layer Chromatography ◽  
Hptlc Method

<p><strong>Objective: </strong>A simple, sensitive, precise, and accurate stability indicating HPTLC (high-performance thin-layer chromatography) method for analysis of 10-gingerol in ginger has been developed and validated as perICH guidelines.</p><p><strong>Methods: </strong>The separation was achieved on TLC (thin layer chromatography) aluminum plates pre-coated with silica gel 60F<sub>254</sub> using n-hexane: ethyl acetate 55:45 (%, v/v) as a mobile phase. Densitometric analysis was performed at 569 nm.</p><p><strong>Results: </strong>This system was found to have a compact spot of 10-gingerol at <em>R</em><sub>F</sub> value of 0.57±0.03. For the proposed procedure, linearity (<em>r</em><sup>2</sup> = 0.998±0.02), limit of detection (18ng/spot), limit of quantification (42 ng/spot), recovery (ranging from 98.35%–100.68%), were found to be satisfactory.</p><p><strong>Conclusion: </strong>Statistical analysis reveals that the content of 10-gingerol in different geographical region varied significantly. The highest and lowest concentration of 10-gingerol in ginger was found to be present in a sample of Patna, Lucknow and Surat respectively which inferred that the variety of ginger found in Patna, Lucknow are much superior to other regions of India.</p>

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