[Simultaneous determination of 21 perfluorinated and polyfluoroalkyl substances in plant oils by ultra-high performance liquid chromatography-triple quadrupole mass spectrometry].

Edible plant oils are a key component of the daily human diet, and the quality and safety of plant oils are related to human health. Perfluorinated and polyfluoroalkyl substances (PFASs) are pollutants that can contaminate plant oil through the processing of raw materials or exposure to materials containing these substances. Thus, establishing a sensitive and accurate analytical method for the determination of PFASs is critical for ensuring the safety of plant oils. In this study, a method based on acetonitrile extraction and solid phase extraction purification combined with ultra-high performance liquid chromatography-triple quadrupole mass spectrometry (UHPLC-MS/MS) was developed for the simultaneous determination of 21 PFASs, including perfluorocarboxylic acids, perfluoroalkyl sulfonic acids, and fluorotelomer sulfonic acids, in edible plant oils. The chromatographic conditions and MS parameters were optimized, and the influences of the extraction solvents and purification method were systematically studied. Plant oil samples were directly extracted with acetonitrile and purified using a weak anion-exchange (WAX) column. The 21 target PFASs were separated on a reversed-phase C18 chromatographic column and detected using a triple quadrupole mass spectrometer with an electrospray ionization source. The mass spectrometer was operated in negative-ion mode. The target compounds were analyzed in multiple reaction monitoring (MRM) mode and quantified using an internal standard method. The results demonstrated that the severe interference observed during the detection of PFASs in the co-extracted substances was completely eliminated after the extraction mixture was purified using a WAX column. The 21 target PFASs showed good linearity in their corresponding ranges, with correlation coefficients greater than 0.995. The limits of detection (LODs) and limits of quantification (LOQs) of the method were in the range of 0.004-0.015 and 0.015-0.050 µg/kg, respectively. The recoveries ranged from 95.6% to 115.8%, with relative standard deviations (RSDs) in the range of 0.3%-10.9% (n=9). The established method is characterized by simple sample pretreatment, good sensitivity, high immunity to interferences, and good stability, rendering it suitable for the rapid analysis and accurate determination of typical PFASs in edible plant oils.

Modifications of Au Nanoparticle-Functionalized Graphene for Sensitive Detection of Sulfanilamide.

In this paper, we present a simple and feasible electrochemical sensor based on Au nanoparticle-functionalized graphene for the determination of sulfanilamide. Au nanoparticles were deposited on graphene, which acted as a platform to prepare excellent nanocomposites. Attributed to the graphene's large surface area and the Au nanoparticles' strong conductivity, many sulfanilamide molecules were enriched on the sensor surface and the signal response became more sensitive. Under the optimal conditions, the electrochemical sensors could be used for the efficient detection of sulfanilamide. Good linearity was observed in the range of 0.1-1000 µmol·L-1 and the detection limit was 0.011 µmol·L-1. Most importantly, the Au nanoparticle-functionalized graphene-modified electrode could be successfully applied for the detection of sulfanilamide in animal meat, and exhibited good stability, acceptable recovery, and offered a promising platform for point-of-care detecting in real samples.

Rapid Detection of Ascorbic Acid Based on a Dual-Electrode Sensor System Using a Powder Microelectrode Embedded with Carboxyl Multi-Walled Carbon Nanotubes.

In this paper, carboxyl groups were introduced by liquid oxidation methods onto multi-walled carbon nanotubes (MWCNTs) to improve the MWCNTs' electrocatalytic properties. A platinum wire microelectrode (ME) was corroded using aqua regia and subsequently embedded with MWCNTs to achieve more active sites, producing a so-called powder microelectrode (PME). Compared with conventional MEs, the PME has a larger specific surface area and more active sites. When PME was used to detect ascorbic acid (AA), the AA oxidation potential shifted negatively and current peak was visibly increased. The calibration curve obtained for AA was in a range of 5.00 × 10-6~9.50 × 10-4 mol·L-1: Ipa(µA) = 3.259 × 10-2+ 1.801 × 10² C (mol·L-1) under the optimum testing conditions. Moreover, the detection and quantitation limits were confirmed at 4.89 × 10-7 mol·L-1 and 1.63 × 10-7 mol·L-1, respectively. When the fabricated PME was practically applied to detect AA, it was shown a recovery rate of 94~107% with relative standard deviation (RSD) <5%. The proposed strategy thus offers a promising, rapid, selective and low-cost approach to effective analysis of AA.