Determination of the alcoholic content in whiskeys using micellar electrokinetic chromatography on microchips.

This report describes the development of a methodology based on micellar electrokinetic chromatography for the separation of alcohols on chip-based systems aiming the determination of alcoholic content in whiskey samples. The separation conditions were optimized the best results were achieved using 50 mmolL-1 phosphate buffer containing 30 mmolL-1 sodium dodecyl sulfate. The alcoholic content was determined in 16 seized whiskey samples from 4 different brands as well as in the original samples. The methodology presented herein allowed the correct classification of 75% of the seized samples as adulterated and the data obtained did not statistically differ from those recorded by a reference technique. The proposed analytical approach emerges as a promising tool to provide a rapid screening of the beverages authenticity and it may be useful to be widely explored for the quality control.

Rapid separation of post-blast explosive residues on glass electrophoresis microchips.

This study describes the development of an analytical methodology based on the use of microchip electrophoresis (ME) devices integrated with capacitively coupled contactless conductivity detection (C4 D) for the separation and detection of inorganic anions in post-blast explosive residues. The best separation condition was achieved using a running buffer composed of 35 mmol/L lactic acid, 10 mmol/L histidine and 0.070 mmol/L cetyl(trimethyl ammonium) bromide. For C4 D measurements, the highest sensitivity was obtained applying a 700 kHz sinusoidal wave with excitation voltage of 20 Vpp . The separation of Cl- , NO3- , NO2- , SO42- , ClO4- and ClO3- was performed within ca. 150 s with baseline resolution and efficiencies between 4.4 × 104 and 1.7 × 105 plates/m. The found limits of detection ranged between 2.5 and 9.5 µmol/L. Last, real samples of post-blast explosive residues were analyzed on the ME-C4 D devices obtaining successfully the determination of Cl- , NO3- and SO42- . The achieved concentration values varied between 12.8-72.5 mg/L for Cl- , 1.7-293.1 mg/L for NO3- and 1.3-201.3 mg/L for SO42- . The data obtained using ME-C4 D devices were in good agreement with the concentrations found by ion chromatography. The approach reported herein has provided short analysis time, instrumental simplicity, good analytical performance and low cost. Furthermore, the ME-C4 D devices emerge as a powerful and portable analytical platform for on-site analysis demonstrating to be a promising tool for the crime scene investigation.

Hydrodynamic injection on electrophoresis microchips using an electronic micropipette.

Here we report for the first time the use of an electronic micropipette as hydrodynamic (HD) injector for microchip electrophoresis (ME) devices. The micropipette was directly coupled to a PDMS device, which had been fabricated in a simple cross format with two auxiliary channels for sample volume splitting. Sample flow during the injection procedure was controlled in automatic dispenser mode using a volume of 0.6µL. Channel width and device configuration were optimized and the best results were achieved using a simple cross layout containing two auxiliary channels with 300µm width for sample splitting. The performance of the HD injector was evaluated using a model mixture of high-mobility cationic species. The results obtained were compared to the data obtained via electrokinetic (EK) injection. Overall, the HD provided better analytical performance in terms of resolution and injection-to-injection repeatability. The relative standard deviation (RSD) values for peak intensities were lower than 5% (n=10) when the micropipette was employed. In comparison with EK injection, the use of the proposed HD injector revealed an unbiased profile for a mixture containing K+ and Li+(300 µmol L-1 each) over various buffer concentrations. For EK injection, the peak areas decreased from 2.92 ± 0.20-0.72 ± 0.14Vs for K+ and from 1.30 ± 0.10-0.38 ± 0.10Vs for Li+ when the running buffer increased from 20 to 50mmolL-1. For HD injection, the peak areas for K+ and Li+ exhibited average values of 2.48±0.07 and 2.10±0.06Vs, respectively. The limits of detection (LDs) for K+, Na+ and Li+ ranged from 18 to 23µmolL-1. HD injection through an electronic micropipette allows to automatically dispense a bias-free amount of sample inside microchannels with acceptable repeatability. The proposed approach also exhibited instrumental simplicity, portability and minimal microfabrication requirements.

Authenticity screening of seized whiskey samples using electrophoresis microchips coupled with contactless conductivity detection.

This report describes for the first time the use of microchip electrophoresis (ME) devices integrated with capacitively coupled contactless conductivity detection (C4 D) to investigate the authenticity of seized whiskey samples, which were probably adulterated by simple dilution with tap water. The proposed microfluidic platform was explored for the monitoring of anionic species (Cl- and F- ) in both original and tampered samples. The best separations were achieved within 70 s using a running buffer composed of lactic acid and histidine (pH = 5.9). ME-C4 D devices were used to analyze samples from three different brands (five samples each). Based on the presence of inorganic anions like Cl- , F- , SO42- and NO2- in different amounts, the authenticity of seized whiskeys was compared to original samples. According to the reported data, the proposed microfluidic platform can be useful to help regulatory authorities in the investigation and monitoring of authenticity of commercialized whiskey beverages.