RESUMO

3D-printing technology has revolutionized electrochemical applications by enabling rapid prototyping of various devices with high precision, even in highly complex structures. However, a significant challenge remains in developing less costly and more sustainable analytical approaches and methods aimed at mitigating the negative environmental impacts of chemical analysis procedures. In this study, we propose a solution to these challenges by creating a simple and versatile electrochemical system that combines 3D-printing technology with recyclable disposable materials, such as graphite from an exhausted battery and a stainless-steel screw. Our results demonstrate a novel strategy for developing electrodes and other laboratory-made devices that align with the principles of sustainability and green chemistry. Furthermore, we provide evidence of the effectiveness of the proposed system in an analytical application involving the simultaneous determination of tert-butylhydroquinone, acetaminophen, and levofloxacin using the voltammetric technique in lake and groundwater samples. The results indicate sufficient accuracy, with recovery values ranging from 91 to 110%. Additionally, we utilized the Analytical GREEnness calculator as a metric system to evaluate the environmental friendliness of the proposed electroanalytical protocol. The final score confirms a favorable level of sustainability, reaffirming the eco-friendly nature of our approach.

RESUMO

Thread-based microfluidic analytical devices have received growing attention since threads have some advantages over other materials. Compared to paper, threads are also capable of spontaneously transporting fluid due to capillary action, but they have superior mechanical strength and do not require hydrophobic barriers. Therefore, thread-based microfluidic devices can be inexpensively fabricated with no need for external pumps or sophisticated microfabrication apparatus. Despite these outstanding features, achieving a controlled and continuous flow rate is still a challenging task, mainly due to fluid evaporation. Here, we overcome this challenge by inserting a cotton thread into a polyethylene tube aiming to minimize fluid evaporation. Also, a cotton piece was inserted into the outlet reservoir to improve the wicking ability of the device. This strategy enabled the fabrication of an innovative electrochemical thread in a tubing microfluidic device that was capable to hold a consistent flow rate (0.38 µL s-1) for prolonged periods, allowing up to 100 injections in a single device by simply replacing the cotton piece in the outlet reservoir. The proposed device displayed satisfactory analytical performance for selected model analytes (dopamine, hydrogen peroxide, and tert-butylhydroquinone), in addition to being successfully used for quantification of nitrite in spiked artificial saliva samples. Beyond the flow rate improvement, this "thread-in-tube" strategy ensured the protection of the fluid from external contamination while making it easier to connect the electrode array to the microchannels. Thus, we envision that the thread in a tube strategy could bring interesting improvements to thread-based microfluidic analytical devices.

Assuntos

RESUMO

In this work, a newly designed electrochemical cell was assembled for in situ integrated microextraction and electroanalysis. Ionic liquids (ILs) were used as extractors to perform the microextraction, which enabled the pre-concentration of norfloxacin from tap water samples. The featured device can be used to replace conventional liquid-liquid microextraction, reducing the number of steps involved in the process. In addition, the pre-concentration of target analyte was performed in a single drop, which was directly decanted onto the electrode surface after agitation, allowing for further determination at trace concentration levels. The analytical performance of the proposed device was evaluated and the norfloxacin was determined at the trace-level in tap water samples with suitable accuracy (recovery values were 86-115%).

RESUMO

A newly configured electrochemical flow cell to be used for (end-channel) amperometric detection in a microfluidic device is presented. The design was assembled to place the reference electrode in a separated compartment, isolated from the flow in the microchannel, while the working and counter electrodes remain in direct contact with both compartments. Moreover, a three-dimensional coil-shaped microfluidic device was fabricated using a nonconventional protocol. Both devices working in association enabled us to solve the drawback caused by the discrete injection when the automatic micropipette was used. The high performance of the proposed electrochemical flow cell was demonstrated after in situ modifying the surface of the platinum working electrode with surfactant (e.g., using Tween 20 at 0.10%). As the reference electrode remained out of contact with the flowing solution, there was no trouble by air bubble formation (generated by accidental insertion or by presence of surfactants) throughout the measurements. This device was characterized regarding its analytical performance by evaluating the amperometric detection of acetaminophen, enabling determination from 6.60 to 66.0 µmol L-1. This issue is important since at high concentration (e.g., as assessed in clinical analysis) the acetaminophen is known to passivate the working electrode surfaces by electrogenerated products, impairing the accuracy of the electrochemical measurements.

RESUMO

The techniques used to monitor the quality of the biodiesel are intensely discussed in the literature, partly because of the different oil sources and their intrinsic physicochemical characteristics. This study aimed to monitor the thermal degradation of the fatty acid methyl esters of Sesamum indicum L. and Raphanus sativus L. biodiesels (SILB and RSLB, resp.). The results showed that both biodiesels present a high content of unsaturated fatty acids, ∼84% (SILB) and ∼90% (RSLB). The SILB had a high content of polyunsaturated linoleic fatty acid (18 : 2), about 49%, and the oleic monounsaturated (18 : 1), ∼34%. On the other hand, RSLB presented a considerable content of linolenic fatty acid (18 : 3), ∼11%. The biodiesel samples were thermal degraded at 110°C for 48 hours, and acid value, UV absorption, and fluorescence spectroscopy analysis were carried out. The results revealed that both absorption and fluorescence presented a correlation with acid value as a function of degradation time by monitoring absorptions at 232 and 270 nm as well as the emission at 424 nm. Although the obtained correlation is not completely linear, a direct correlation was observed in both cases, revealing that both properties can be potentially used for monitoring the biodiesel degradation.

RESUMO

A procedure based on liquid-liquid extraction (LLE) and phase separation using magnetically stirred salt-induced high-temperature liquid-liquid extraction (PS-MSSI-HT-LLE) was developed to extract and pre-concentrate ciprofloxacin (CIPRO) and enrofloxacin (ENRO) from animal food samples before electroanalysis. Firstly, simple LLE was used to extract the fluoroquinolones (FQs) from animal food samples, in which dilution was performed to reduce interference effects to below a tolerable threshold. Then, adapted PS-MSSI-HT-LLE protocols allowed re-extraction and further pre-concentration of target analytes in the diluted acid samples for simultaneous electrochemical quantification at low concentration levels. To improve the peak separation, in simultaneous detection, a baseline-corrected second-order derivative approach was processed. These approaches allowed quantification of target FQs from animal food samples spiked at levels of 0.80 to 2.00 µmol L-1 in chicken meat, with recovery values always higher than 80.5%, as well as in milk samples spiked at 4.00 µmol L-1, with recovery values close to 70.0%.

Assuntos

RESUMO

A baseline-corrected second-order derivative procedure and a miniaturized sample preparation based on low-density solvent and ultrasound-assisted liquid-liquid microextraction (LDS-UA-LLME) was combined to provide the simultaneous electroanalysis of three fluoroquinolones (FQ) as emerging contaminants (ECs). The enhanced mathematical processing provided the best separation with an accurate measurement of the overlapping peaks during the simultaneous electro-oxidation of target FQs that were directly dropped on the surface of carbon nanofiber-modified screen-printed electrodes. The adapted LDS-UA-LLME protocol was the key step involved in the sample preparation, which preconcentrate target analytes from diluted tap water samples with an enrichment factor of around 80×, allowing their quantification at trace levels. This combined feature demonstrated the unique application of an electroanalytical technique for the simultaneous electroanalysis of three FQs in spiked tap water samples, with recovery values remarkably close to 100%.

Assuntos

RESUMO

This paper introduces a simple, fast and reliable electroanalytical method for differential-pulse polarography based on electrochemical reduction at a dropping mercury electrode. The method was validated for the determination of 2-ethylhexyl-4-methoxycinnamate (EHMC) alone and in association with 4-methylbenzylidene camphor (MBC) or 2-hydroxy-4-methoxybenzophenone (BENZ-3) in samples of commercial cosmetic preparations. The supporting electrolyte that provided the best-defined and most intense peak current for EHMC determination was Britton-Robinson buffer (pH 4.0) in the presence of a cationic surfactant. Under optimized conditions, EHMC exhibited one single peak of reduction at -1.49 V versus Ag/AgCl. A limit of detection of 3.76 x 10(-8)mol L(-1) and a limit of quantitation of 1.25 x 10(-7) mol L(-1) were found for the pure EHMC standard. A good average recovery rate was reached for all the samples analyzed.