Combination Of Liquid-phase Microextraction Research Articles

Sensitive determination of nickel at trace levels in surface water samples by slotted quartz tube flame atomic absorption spectrometry after switchable solvent liquid-phase microextraction.

In this study, switchable solvent (SS) for liquid-phase microextraction (LPME) was used as a tool to preconcentrate nickel from aqueous samples for determination by flame atomic absorption spectrometry. The SS-LPME method was optimized thoroughly to boost the absorbance signal of nickel for trace level determination. Parameters optimized included switchable solvent volume, sodium hydroxide concentration, sodium hydroxide volume, and eluent volume. The SS-LPME method enhanced the detection power by about 32-folds, and a slotted quartz tube (SQT) was used to obtain 2.6-folds increase in detection power. The combination of LPME and SQT-FAAS produced 104-folds enhancement, correlating to a limit of detection value of 1.8μg/L. Low relative standard deviations calculated for the lowest calibration concentration indicated good repeatability for replicate measurements. Accuracy of the optimized method and its applicability to real samples was tested on two river samples. The results (85-103%) obtained from the spike recovery experiments were satisfactory.

Study of the mechanism of acetonitrile stacking and its application for directly combining liquid-phase microextraction with micellar electrokinetic chromatography

Acetonitrile stacking is an online concentration method that is distinctive due to its inclusion of a high proportion of organic solvent in sample matrices. We previously designed a universal methodology for the combination of liquid-phase microextraction (LPME) and capillary electrophoresis (CE) using acetonitrile stacking and micellar electrokinetic chromatography (MEKC) mode, thereby achieving large-volume injection of the diluted LPME extractant and the online concentration. In this report, the methodology was extended to the analysis of highly substituted hydrophobic chlorophenols in wines using diethyl carbonate as the extractant. Additionally, the mechanism of acetonitrile stacking was studied. The results indicated that the combination of LPME and MEKC exhibited good analytical performance: with ∼40-fold concentration by LPME, a 20-cm (33% of the total length) sample plug injection of an eight-fold dilution of diethyl carbonate with the organic solvent-saline solution produced enrichments higher by a factor of 260–791. Limits of qualification ranged from 5.5 to 16.0ng/mL. Acceptable reproducibilities of lower than 1.8% for migration time and 8.6% for peak areas were obtained. A dual stacking mechanism of acetonitrile stacking was revealed, involving transient isotachophoresis plus pH-junction stacking. The latter was associated with a pH shift induced by the presence of acetonitrile. The pseudo-stationary phase (Brij-35) played an important role in reducing the CE running time by weakening the isotachophoretic migration of the analyte ions following Cl− ions. The combination of acetonitrile stacking and nonionic micelle-based MEKC appears to be a perfect match for introducing water-immiscible LPME extractants into an aqueous CE system and can thus significantly expand the application of LPME-CE in green analytical chemistry.

Separation and Determination of Amitriptyline and Nortriptyline in Biological Samples Using Single-Drop Microextraction with GC

The combination of liquid phase microextraction (LPME) based on a single drop and gas chromatography flame ionization detector (GC-FID) was used for separation and determination of amitriptyline and nortriptyline in human plasma and urine samples. The sample solution was kept alkaline (pH 12), then a microdrop of organic solvent (isooctane) was suspended in the donor solution; after extraction, the organic microdrop was injected into the GC-FID. Experimental LPME conditions were optimized. Finally, the enrichment factors (89.5–139.0), the relative standard deviation (RSD%, n = 5) 1.1–8.5, linearity ranges (0.05–20 μg mL−1), and the limits of detections (0.01, 0.02 μg mL−1) for selected drugs were evaluated.

Determination of iodate in waters by cuvetteless UV–vis micro-spectrophotometry after liquid-phase microextraction

The combination of liquid-phase microextraction and microvolume UV-vis spectrophotometry has been applied to the determination of iodate in natural water samples. The method is based on the reduction of iodate into vapor iodine and extraction of this volatile onto a single drop of N,N'-dimethylformamide. The following derivatization reaction was employed: Optimum conditions employed for iodate determination were as follows: 2.5 microL N,N'-dimethylformamide exposed to the headspace of a 10 mL acidic (HCl 0.2 mol L(-1)) aqueous solution stirred at 1400 rpm for 7 min after addition of 1 mL of KI 10(-3)mol L(-1) for in situ iodine generation. The limit of detection was determined as 1.1 microg L(-1). The repeatability, expressed as relative standard deviation, was 4.2% (n=6). A large preconcentration factor (i.e. 396) was obtained in only 7 min.

Combination of liquid-phase microextraction and on-column stacking for trace analysis of amino alcohols by capillary electrophoresis.

We described a new method for the enrichment of basic drugs present in water samples via liquid-phase microextraction (LPME) combined with on-column stacking in capillary electrophoresis. Two steps were employed to enhance the detection sensitivity of four amino alcohols. The analytes were first extracted from aqueous sample (donor solution) that were adjusted to basic through a thin layer of 1-octanol entrapped within the pores of a polypropylene hollow fiber, and then into a 5-microl acidic acceptor solution inside the hollow fiber. The extract was then further enriched through on-column stacking in capillary electrophoresis. With this two-step enrichment procedure, the method provided 72-110-fold preconcentration of the target amino alcohols. The limits of detection were 0.08-0.5 microg/ml. Relative standard deviation (n=6) ranged between 4.3 and 6.9% for the studied drugs utilizing 2-amino-1-phenylethanol as internal standard. The extraction of amino alcohols in spiked urine samples was evaluated using the developed procedure.