Development of a Liquid-Phase Microextraction Method Prior to HPLC Analysis of Quercetin in Food Samples.

In this research, an efficient, fast, low-cost and easy-to-use liquid-phase microextraction method was established to measure quercetin in onion and tomato before analysis by HPLC instrument. Herein, a rotatable central composite design-response surface methodology and artificial neural network were applied to model, optimize and predict the affecting factors on the microextraction procedure. Here, a minimal level of extractant was applied in the absence of a disperser. The cloudy state was formed by repeatedly suctioning and injecting the mixture of the aqueous solution and extractant with a glass syringe. Due to this procedure, a turbid solution composed of the very fine droplets of extractant dispersed in the aqueous solution was created, the contact surface was significantly enlarged and the quercetin was promptly extracted. The optimum values for the proposed method included 284 µL of 1-undecanol as the organic extractive solvent, pH of sample 3.3, the number of air injected nine times and speed and duration of centrifugation 4,000 rpm and 5 min. The linear range and detection of limit were achieved at 20-4,000 and 6 µg L-1, respectively. RSD% was obtained ˂4.93% (n = 5). This model was applied to monitor quercetin in tomato and onion samples.

Application of Taguchi L16 design method for comparative study of ability of 3A zeolite in removal of Rhodamine B and Malachite green from environmental water samples.

This study aimed to investigate the efficiency of 3A zeolite as a novel adsorbent for removal of Rhodamine B and Malachite green dyes from water samples. To increase the removal efficiency, effecting parameters on adsorption process were investigated and optimized by adopting Taguchi design of experiments approach. The percentage contribution of each parameter on the removal of Rhodamine B and Malachite green dyes determined using ANOVA and showed that the most effective parameters in removal of RhB and MG by 3A zeolite are initial concentration of dye and pH, respectively. Under optimized condition, the amount predicted by Taguchi design method and the value obtained experimentally, showed good closeness (more than 94.86%). Good adsorption efficiency obtained for proposed methods indicates that, the 3A zeolite is capable to remove the significant amounts of Rhodamine B and Malachite green from environmental water samples.

Application of response surface methodology for air assisted-dispersive liquid- liquid microextraction of deoxynivalenol in rice samples prior to HPLC-DAD analysis and comparison with solid phase extraction cleanup.

A fast, simple, and easy to operate air assisted-dispersive liquid-liquid microextraction (AA-DLLME) for preconcentration and extraction of deoxynivalenol (DON) from rice samples is proposed and compared with solid phase extraction (SPE) cleanup. DON was determined using a high performance liquid chromatography with diode-array detection (HPLC-DAD). AA-DLLME was performed using a glass syringe and dispersion of extractant in the sample solution was achieved with help of air bubbles. Chloroform was used as the extractant solvent. To find out the optimized condition for the proposed method, response surface methodology (RSM) was applied for multivariate optimization of effecting parameters namely volume of extractant, number of extraction, pH, and rate of centrifugation. Under optimized condition the dynamic range of calibration graph was found to be 50-500µgL-1 with detection limit of 23.6µgL-1. Both methods were applied for extraction of DON from rice.

Application of In-Syringe Dispersive Liquid-Liquid Microextraction Coupled to GC/FID for Determination of Trace Contamination of Phthalate Esters in Water Samples.

In this work, a simple and easy to handle one-step in-syringe setup for the dispersive liquid-liquid microextraction method has been developed for preconcentration of trace quantities of four kinds of phthalate esters (PEs) in water samples as a prior step to its determination by gas chromatography/flame ionization detector. The environmental pollution at this method has been limited due to using a glass syringe as extraction unit and also a very small amount of n-hexane as a safe solvent. Some important parameters such as the type of extraction and disperser solvents, extraction and disperser solvents volume, sample volume and ionic strength were investigated and optimized. Validation experiments showed that the optimized method had precision (1.7-6.9%) and high recovery (94.32-104.7%), and the limits of detection were from 0.406 to 1.33 µg L(-1). At the end, the method was successfully applied for the determination of PEs in real water samples.

Application of In-Syringe Dispersive Liquid-Liquid Microextraction and Narrow-Bore Tube Dispersive Liquid-Liquid Microextraction for the Determination of Trace Amounts of BTEX in Water Samples.

Two new simple and effective methods based on dispersive liquid-liquid microextraction (DLLME) procedure, termed "in-syringe DLLME (IS-DLLME)" and "narrow-bore tube DLLME (NB-DLLME)", were developed and applied for rapid and simultaneous separation and preconcentration of trace amounts of benzene, toluene, ethylbenzene and xylene isomers in water samples followed by gas chromatographic analysis. Different parameters influencing the extraction efficiency of both methods such as type and volume of the extraction solvent and the disperser solvent; pH, temperature and volume of sample solution and ionic strength of samples were investigated and optimized. Under optimal condition, the limits of detection ranged from 1.7 to 2.4 µg L(-1) for IS-DLLME and 1.5 to 2.2 µg L(-1) for NB-DLLME. Precision (as relative standard deviation) of the two techniques was between 2.1 and 4.6% for IS-DLLME and between 1.5 and 4.5% for NB-DLLME. The enrichment factors found to be between 20-29 and 31-73 for IS- and NB-DLLME, respectively. The applicability of the proposed methods was investigated by analyzing real water samples.

Headspace liquid phase microextraction for quantitation of hexanal in potato crisps by gas chromatography.

A simple and rapid method using headspace liquid-phase microextraction (HS-LPME) was developed for the determination of hexanal at low levels in potato crisp samples. Parameters such as extraction solvent, agitation of the sample, salt addition, organic drop volume, exposure time, and extraction time were controlled and optimised. The developed protocol was found to yield a linear calibration curve in the concentration range from 0.001 to 2 mg/L and a limit of detection of 0.1 microg/L with a good enrichment factor of > 107 for the analyte. The repeatability of the method was satisfactory (4%). The results demonstrate that HS-LPME is a rapid, accurate, and effective preparation method and could be successfully used for the determination of hexanal in potato crisp samples.