Ringer Tablet-Based Micelle-Mediated Extraction-Solvent Back Extraction Coupled with High-Performance Liquid Chromatography for Preconcentration and Determination of Neonicotinoid Pesticides

Author(s):  
Jitlada Vichapong ◽  
Rawikan Kachangoon ◽  
Rodjana Burakham ◽  
Yanawath Santaladchaiyakit ◽  
Supalax Srijaranai
2013 ◽  
Vol 33 (8) ◽  
pp. 863-872 ◽  
Author(s):  
Alireza Asghari ◽  
Hamidreza Fazl-Karimi ◽  
Behruz Barfi ◽  
Maryam Rajabi ◽  
Ali Daneshfar

Aminophenol isomers (2-, 3-, and 4-aminophenols) are typically classified as industrial pollutants with genotoxic and mutagenic effects due to their easy penetration through the skin and membranes of human, animals, and plants. In the present study, a simple and efficient ultrasound-assisted emulsification microextraction procedure coupled with high-performance liquid chromatography with ultraviolet detector was developed for preconcentration and determination of these compounds in human fluid and environmental water samples. Effective parameters (such as type and volume of extraction solvent, pH and ionic strength of sample, and ultrasonication and centrifuging time) were investigated and optimized. Under optimum conditions (including sample volume: 5 mL; extraction solvent: chloroform, 80 µL; pH: 6.5; without salt addition; ultrasonication: 3.5 min; and centrifuging time: 3 min, 5000 rpm min−1), the enrichment factors and limits of detection were ranged from 42 to 51 and 0.028 to 0.112 µg mL−1, respectively. Once optimized, analytical performance of the method was studied in terms of linearity (0.085–157 µg mL−1, r2 > 0.998), accuracy (recovery = 88.6– 101.7%), and precision (repeatability: intraday precision < 3.98%, and interday precision < 5.12%). Finally, applicability of the method was evaluated by the extraction and determination of these compounds in human urine, hair dye, and real water samples.


2014 ◽  
Vol 10 (4) ◽  
pp. 2654-2660
Author(s):  
Sylwia Magiera ◽  
PhD Weronika Adolf ◽  
Prof. Irena Baranowska

A novel high performance liquid chromatography with fluorescence detector (HPLC-FL) method for determination of metoprolol enantiomers in a pharmaceutical formulation was developed and validated. This study investigated the ultrasound-assisted extraction (UAE) of metoprolol from commercial tablets using methanol as extraction solvent. The separation of enantiomers was successfully carried out with a CHIRALCEL OD-RH column, under isocratic elution mode using 0.05% trifluoroacetic acid and 0.05% diethylamine in water and acetonitrile (80:20, v/v).The chromatographic method was validated in terms of precision, accuracy, detection and quantification limits, linearity and recovery. Calibration curves were linear in the investigated range with correlation coefficient better than 0.9931 while the limit of quantifications was 0.19 µg mL-1 for S(–)-MET and 0.23 µg mL-1 for R(+)-MET. The mean recovery of S(–)-MET and R(+)-MET from tablets were found to be 78.8% and 92.1%, respectively.This method for the direct determination and quantification of metoprolol enantiomers in pharmaceutical formulations is suitable for routine analyses in quality control laboratories and was applied to evaluate for the first time, the presence and the quantities of cited analytes in commercially available formulation. 


Talanta ◽  
2016 ◽  
Vol 161 ◽  
pp. 398-404 ◽  
Author(s):  
Anas Alshishani ◽  
Ahmad Makahleh ◽  
Hui Fang Yap ◽  
Elbaleeq Adam Gubartallah ◽  
Salizawati Muhamad Salhimi ◽  
...  

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