Sequential Injection Analysis for Rapid Determination of Mercury in Skincare Products Based on Fluorescence Quenching of Eco-Friendly Synthesized Carbon Dots.

This work reports the analysis of mercury using a spectrofluorometric method combined with a sequential injection analysis (SIA) system. This method is based on the measurement of fluorescence intensity of carbon dots (CDs), which is quenched proportionally after adding mercury ions. Herein, the CDs underwent environmentally friendly synthesis using a microwave-assisted approach that provides intensive and efficient energy and shortens reaction time. After irradiation at 750 W for 5 min in a microwave oven, a dark brown CD solution with a concentration of 2.7 mg mL-1 was obtained. The properties of the CDs were characterized by transmission electron microscopy, X-ray diffractometry, X-ray photoelectron spectroscopy, Fourier-transform infrared spectroscopy, and UV-vis spectrometry. We presented for the first time the use of CDs as a specific reagent for the determination of mercury in skincare products with the SIA system to achieve rapid analysis and full automatic control. The as-prepared CD stock solution was diluted 10 times and used as a reagent in the SIA system. Excitation and emission wavelengths at 360 and 452 nm, respectively, were used to construct a calibration curve. Physical parameters affecting the SIA performance were optimized. In addition, the effect of pH and other ions was investigated. Under the optimum conditions, our method showed a linear range from 0.3 to 600 mg L-1 with an R 2 of 0.99. The limit of detection was 0.1 mg L-1. Relative standard deviation was 1.53% (n = 12) with a high sample throughput of 20 samples per hour. Finally, the accuracy of our method was validated by comparison using inductively coupled plasma mass spectrometry. Acceptable recoveries were also presented without a significant matrix effect. This method was also the first time that uses the untreated CDs for the determination of mercury(II) in skincare products. Therefore, this method could be an alternative for mercuric toxic control in other sample applications.

Simple Portable Voltammetric Sensor Using Anodized Screen-Printed Graphene Electrode for the Quantitative Analysis of p-Hydroxybenzoic Acid in Cosmetics.

Screen-printed graphene electrodes (SPGEs) have become a potential option in electrochemical applications because of their outstanding properties and disposable approach to miniaturize the electrodes for onsite analysis. Herein, the detection of para-hydroxybenzoic acid (PHBA) in cosmetics using the anodized SPGE has been pioneered and reported. The simple anodization of the SPGE surface was operated by anodic pretreatment at a constant potential on SPGE. The surface morphologies and electrochemical behaviors of anodized SPGEs in different anodization electrolytes were examined. Using anodized SPGE in a phosphate-buffered solution, a nontoxic solution, the sensitivity of PHBA detection was significantly improved compared with pristine SPGE owing to the increase of the polar oxygen-containing functional group during the anodization. The anodized SPGE could detect a PHBA down to 0.073 µmol/L. Finally, the developed anodized SPGE presented high ability and feasibility for PHBA detection in cosmetics. Furthermore, a facile electrode preparation step with a nontoxic solution can present high reproducibility and compatibility with a portable potentiostat for onsite PHBA detection during manufacturing.

Simultaneous and direct determination of urea and creatinine in human urine using a cost-effective flow injection system equipped with in-house contactless conductivity detector and LED colorimeter.

This work presents a cost-effective and simple flow injection analysis (FIA) system for simultaneous and direct determination of urea and creatinine in human urine. The FIA system comprises two in-house detectors, a contactless conductivity detector and a light emitting diode (LED) detector. The contactless detector was built as a flow-through detection cell with axial electrodes, commonly known as capacitively coupled contactless conductivity detector (C4D) and the diode detector was fabricated based on the concept of paired emitter detector diodes (PEDD). With appropriate dilution of urine, the sample is directly injected into a stream of glycine-NaOH buffer pH 8.8 (the gas donor stream) and is carried by the carrier through a urease minicolumn for on-line enzymatic hydrolysis. The generated NH3 diffuses from the carrier stream through a porous polytetrafluoroethylene (PTFE) membrane into a stream of deionized water (the acceptor stream) leading to an increase in the signal at the C4D due to the NH3 dissolution in the water. In this system, creatinine is determined based on the Jaffé reaction by merging a stream of alkaline picrate with the gas donor stream. The change in color is detected using the PEDD equipped with two green LEDs. Under the optimum condition, the linear range of urea and creatinine were 30-240 mg L-1 and 10-500 mg L-1, with limits of detection of 9.0 mg L-1 and 0.9 mg L-1, respectively. The proposed system provides satisfactorily good precision (RSD < 3%), with sample throughput of 31 sample h-1 for the two analytes. The FIA system tolerates potential interference commonly found in human urine. The system was successfully applied and validated with selected reference methods.

Simultaneous Colorimetric Measurements of Antioxidant Capacity by Flow Injection Analysis with Paired Emitter Detector Diode.

An effective flow injection analysis (FIA) system employing paired emitter detector diode (PEDD) for simultaneous dual antioxidant assays is proposed. The total antioxidant capacity (TAC) was measured using the 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) assay in parallel with the ferric reducing antioxidant power (FRAP) assay. Ascorbic acid was used as the reference antioxidant and the TAC value reported as ascorbic acid equivalent (AAE). A 10-port valve furnished with two injection loops allowed the sample from one loop to react with the ABTS reagent and be detected by one PEDD. At the same time, the sample from the second loop reacted with the FRAP reagent and is detected at the second PEDD. A pair of red light emitting diodes (634 nm) was employed for both PEDDs. The linearity range was 10 to 50 µM ascorbic acid, with limit of detection of 3.18 and 4.37 µM, and precision of 2.41 and 2.15% RSD (for 30 µM ascorbic acid, n = 10) for the ABTS and FRAP assay, respectively. Sample throughput of 90 samples/h was achieved. The method was applied to the measurement of TAC of commercial fruit juice, instant tea products and vitamin C tablets. The observed AAE values were in good agreement with those obtained using batch methods with a spectrophotometer.

Green analytical method for simultaneous determination of salinity, carbonate and ammoniacal nitrogen in waters using flow injection coupled dual-channel C4D.

A flow injection analysis system (FIA) for the simultaneous determination of salinity, carbonate and ammoniacal nitrogen has been developed and reported in this paper. FIA incorporating membrane units was used, not only for the separation of the gaseous carbon dioxide and ammonia, but also for on-line dilution in the salinity measurement. The sample was injected via a 10-port valve with two sample loops. One loop was used for salinity and carbonate measurements and the second loop for ammoniacal nitrogen determination. A dual-channel capacitively coupled contactless conductivity detector was assembled in a single shielding box. Input voltage from the same AC power supply was fed to the input electrodes of both C4D cells. One channel of the C4D was used to monitor the change in conductivity of an acceptor stream that carried a zone of the water sample that has passed through the on-line dilution unit. Conductivity of this zone relates directly to the salinity of the sample. The same sample zone was next acidified to generate carbon dioxide gas that diffused through a hydrophobic membrane of the first gas diffusion (GD) unit. The zone of dissolved carbon dioxide in acceptor stream of water flowed into the same C4D cell as for the salinity measurement, but arriving at a later time. Concurrently, the second channel of the C4D monitored the change in conductivity of the acceptor stream in the second GD unit due to the diffusion of ammonia gas generated by the reaction of base with the sample injected from the second sample loop. The change in conductivity at this second C4D cell correlates with the concentration of ammoniacal nitrogen present in the sample. The proposed method is low cost, simple, rapid and sensitive. The limit of quantitation for salinity, carbonate and ammoniacal nitrogen are 0.31mmolL-1, 1.85 µmol L-1, respectively. Throughput of 20 samples h-1 for simultaneous analysis can be achieved with RSD of less than 3.8%. The system had been applied to the determination of salinity, carbonate and ammoniacal nitrogen in 15 water samples, with results in agreement with those obtained using comparison methods.

Poly(vinyl alcohol) capped silver nanoparticles for antioxidant assay based on seed-mediated nanoparticle growth.

A simple and rapid method for measurement of total antioxidant capacity (TAC) was developed. In this work, gallic acid was used as the antioxidant standard. Poly(vinyl alcohol) embedded silver nanoparticles (PVA-AgNPs) were employed as a colorimetric sensor. The detection principle was based on the seed-mediated nanoparticle growth technique. The PVA-AgNPs act as a catalyst in the reduction of Ag+ by gallic acid by providing nucleation seeds. Ag+ was reduced to Ag° and accumulated on the PVA-AgNP surface, leading to an increase in the size of particles. The absorbance of the colloidal solution was drastically enhanced with a small red shift. Under optimal conditions, a linear response was established between the change in absorbance and the TAC value expressed in terms of gallic acid equivalents. The linear range was from 25 to 200µM with a detection limit of 22.1µM. Satisfactory precision was obtained with % relative standard deviation (RSD) of 2.17. The developed sensor was successfully applied for TAC assessment of commercial ginger products. The PVA-AgNP sensor offers rapid analysis (within 5min) compared to other nanoparticle-based antioxidant assays. Synthesis of the particles and assay involved less-toxic chemicals, and is therefore a "greener" method.