Sharif Digital Repository

A simple and rapid method for simultaneous separation and preconcentration of ultra-trace amounts of nitrate and nitrite using in-syringe liquid microextraction is developed. The extraction procedure is based on the selective ion-pairing complex formation of nitrate and nitrite with Cu(I)-neocuproine in 100 μL of 1-butyl-3-methylimidazolium hexafluorophosphate as an extracting phase within a syringe. The atomic-absorption signal of copper in the ionic liquid layer is proportional to the nitrate and nitrite concentrations. When barbituric acid is used, nitrite is converted into violuric acid and thus it is removed from the environment. In this case, the selectivity of the modified-ligand is... 

A horizontally oriented liquid-liquid-liquid microextraction (HOLLLME) setup was developed and applied for the isolation of two major estrogens from aquatic media. In contrast to the conventional procedure, in this setup the extracting microdrop was suspended from a horizontally positioned needle in order to provide much higher stability to the extracting phase. The developed HOLLLME approach was applied to isolate two major selected estrogens from aquatic media followed by high performance liquid chromatography-ultraviolet (HPLC-UV) determination. Estrogens were, initially, extracted from water samples into hexane and subsequently, the back extraction stage was performed with 6 μL of sodium... 

A multi-residue method using gas chromatography coupled with flame ionisation detector has been developed for simultaneous determination of 10 pesticides in milk. The methodology involved a sample clean-up procedure using ‘quick, easy, cheap, effective, rugged and safe’ followed by a preconcentration step based on dispersive liquid–liquid microextraction. In this regard, acetonitrile was added to the milk sample with specific pH and ionic strength, and the mixture was rigorously shaken. The extracts were centrifuged; then, the organic phase (acetonitrile) was transferred to a test tube and was mixed with deionised water. The mixture was sonicated and chloroform was added as an acceptor phase... 

A multi-residue method using gas chromatography coupled with flame ionisation detector has been developed for simultaneous determination of 10 pesticides in milk. The methodology involved a sample clean-up procedure using ‘quick, easy, cheap, effective, rugged and safe’ followed by a preconcentration step based on dispersive liquid–liquid microextraction. In this regard, acetonitrile was added to the milk sample with specific pH and ionic strength, and the mixture was rigorously shaken. The extracts were centrifuged; then, the organic phase (acetonitrile) was transferred to a test tube and was mixed with deionised water. The mixture was sonicated and chloroform was added as an acceptor phase... 

Experimental design of directly suspended droplet liquid-liquid-liquid microextraction has been used to determine residue of 2,4-D, in environmental water samples. A free suspended droplet of 5.5 μL of receiving phase is delivered to the top-center position of 1-Octanol, which is an immiscible organic solvent, floating on the top of a 2.5 mL aqueous sample while being agitated by a stirring bar to create a mild vortex at the center of the vial. Central composite rotatable design has been used for studying the effect of the parameters, the factors interacting with each other and finding the optimum condition. The chromatographic separation was accomplished on a shim-Pak C18 column using a... 

Multivariate curve resolution-alternating least squares (MCR-ALS) as a second-order calibration algorithm was proposed for the simultaneous analysis of eighteen fatty acid methyl esters (FAMEs) in a standard mixture and pomegranate seed sample using vortex-assisted extraction-dispersive liquid-liquid microextraction (VAE-DLLME), followed by gas chromatography-mass spectrometry (GC-MS). The chemometric resolution, identification and quantification of the target FAMEs in the standard mixture and real sample (i.e., the pomegranate seed) were carried out successfully in the presence of some uncalibrated interferences. The lack of fit (LOF) and reverse match factor (RMF) were used for the... 

Dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-mass spectrometry-selective ion monitoring (GC-MS-SIM) was applied to the determination of methyl tert-butyl ether (MTBE) in water samples. The effect of main parameters affecting the extraction efficiency was studied simultaneously. From selected parameters, volume of extraction solvent, volume of dispersive solvent, and salt concentration were optimized by means of experimental design. The statistical parameters of the derived model were R 2=0.9987 and F=17.83. The optimal conditions were 42.0μL for extraction solvent, 0.30mL for disperser solvent and 5% (w/v) for sodium chloride. The calibration linear range... 

In this study, QuEChERS combined with dispersive liquid-liquid microextraction is developed for extraction of ten pesticides in complex sample matrices of water and milk. In this regard, effective factors of proposed extraction technique combined with gas chromatography with flame ionization detector were designed, modeled, and optimized using central composite design, multiple linear regression, and Nelder–Mead simplex optimization. Later, univariate calibration model for ten pesticides was developed in concentration range of 0.5–100 ng/mL. Surprisingly, quadratic calibration behavior was observed for some of the pesticides. In this regard, Mandel's test was used for evaluating linearity... 

Liquid-liquid-liquid microextraction (LLLME) in combination with HPLC and UV detection has been used as a sensitive method for the determination of ephedrine in urine samples. Extraction process was performed in a homemade total glass vial without using a Teflon ring, usually employed. Ephedrine was first extracted from 3.5 mL of urine sample (pH 12) into a microfilm of toluene/benzene (50:50). The analyte was subsequently back extracted into an acidic microdrop solution (pH 2) suspended in the organic phase. The extract was then injected into the HPLC system directly. An enrichment factor of 137 along with a good sample clean-up was obtained under the optimized conditions. The calibration...