Malathion, phoxim, and thiram are organophosphates and organosulfur pesticides widely used in agricultural products. The residues of these pesticides present a direct threat to human health. Rapid and on-site detection is critical for minimizing such risks. In this work, a simple approach was introduced using a flexible surface-enhanced Raman spectroscopy (SERS) substrate. The prepared Ag nanoparticles-polydimethylsiloxane (AgNPs-PDMS) substrate showed high SERS activity, good precision (relative standard deviation = 5.33%), and stability (30 days) after optimization. For target pesticides, the linear relationship between characteristic SERS bands and concentrations were achieved in the range of 10~1000, 100~5000, and 50~5000 μg L⁻¹ with LODs down to 3.62, 41.46, and 15.69 μg L⁻¹ for thiram, malathion, and phoxim, respectively. Moreover, SERS spectra of mixed samples indicated that three pesticides can be identified simultaneously, with recovery rates between 96.5 ± 3.3% and 118.9 ± 2.4%, thus providing an ideal platform for detecting more than one target. Pesticide residues on orange surfaces can be simply determined through swabbing with the flexible substrate before acquiring the SERS signal. This study demonstrated that the prepared substrate can be used for the rapid detection of pesticides on real samples. Overall, this method greatly simplified the pre-treatment procedure, thus serving as a promising analytical tool for rapid and nondestructive screening of malathion, phoxim, and thiram on various agricultural products.

This study introduces a novel method for detecting free glycidol and total free monochloropropanediol (MCPD) in fish and krill oil. Before analysis on high-performance liquid chromatography–tandem mass spectrometry (HPLC-MS), p-(dimethylamino)phenol was used for derivatization of these compounds, enabling the sensitive determination of these contaminants. The sample preparation procedure includes a simple, efficient pretreatment using NaCl aqueous solution extraction and C18 sorbent cleanup (for demulsification), distinguishing glycidol from MCPD under varied reaction conditions for derivatization (weak acidic and strong alkaline aqueous environments). This approach shows broad linearity from 1 to at least 256 ng·mL⁻¹, improved sensitivity compared to standard GC-MS methods, with the limit of detection (LOD) and limit of quantification (LOQ) for MCPD and glycidol in both oil samples verified at 0.5 ng·mL⁻¹ and 1 ng·mL⁻¹, respectively. Different from previous HPLC-MS methods for direct detection of glycidol esters or MCPD esters, this is the first HPLC-MS method used for the detection of free glycidol and total free MCPD in edible oil. Furthermore, this method can be potentially developed for glycidol or monochloropropane diol esters, which is similar to the current official methods adopted for indirect detection of these contaminants in different food matrices. Application of this detection method to real dietary supplements (fish oil and krill oil) revealed MCPD residues in fish oil (maximum detected: 32.78 ng·mL⁻¹) and both MCPD (maximum detected: 2767.3 ng·mL⁻¹) and glycidol (maximum detected: 22.2 ng·mL⁻¹) in krill oil, emphasizing its effectiveness and accuracy for assessing contamination in these supplements.

Malachite green (MG) is a synthetic poisonous organic compound that has been banned in many countries as a veterinary drug for aquaculture. An efficient, fast and sensitive method is urgently needed for monitoring the illegal use of malachite green (MG) in aquaculture. In this study, a novel ratiometric fluorescence immunoassay was established. Nitrogen-doped carbon quantum dots were used as ratiometric fluorescent probes with a fluorescence peak at 450 nm. Horseradish peroxidase was employed to convert o-phenylenediamine to 2,3-diaminophenazine, with a new fluorescence peak at 580 nm and a strong absorption at 420 nm. The inner filter effect between N-CQD fluorescence and DAP absorption was identified. It allows for the ratiometric detection of MG using a fluorescent immunoassay. The results demonstrated a linear ratiometric fluorescence response for MG between 0.1 and 12.8 ng·mL⁻¹. The limit of detection of this method was verified to be 0.097 μg·kg⁻¹ with recoveries ranging from 81.88 to 108%, and the relative standard deviations were below 3%. Furthermore, this method exhibited acceptable consistency with the LC-MS/MS results when applied for MG screening in real samples. These results demonstrated a promising application of this novel ratiometric fluorescence immunoassay for MG screening with the merits of rapid detection, simple sample preparation, and stable signal readout. It can be an alternative to other traditional methods if there are difficulties in the availability of expensive instruments, and achieve comparable results or even more sensitivity than other reported methods.

In this work, a novel method for the colorimetric sensing of α-glucosidase (α-Glu) activity was developed based on CoOOH nanoflakes (NFs), which exhibit efficient oxidase-mimicking activity. Colorless 3,3′,5,5′-tetramethylbenzidine (TMB) can be oxidized by CoOOH NFs into blue-colored oxidized TMB (oxTMB) in the absence of H₂O₂. L-Ascorbic acid-2-O-α-D-glucopyranose (AAG) can be hydrolysed by α-glucosidase to produce ascorbic acid, resulting in a significant decrease of catalytic activity of CoOOH NFs. Thus, a colorimetric α-glucosidase activity detection method was designed with a limit of detection of 0.0048 U mL⁻¹. Furthermore, the designed sensing platform exhibits favorable applicability for the α-glucosidase (α-Glu) activity assay in real samples. Meanwhile, this method can be expanded to study the inhibitors of α-Glu. Finally, the as-proposed method combined with a smartphone would be a color recognizer, which was successfully applied for the determination of α-Glu activity in human serum samples.

Pesticide residues in aquatic products are of great concern due to the risk of environmental transmission and their extensive use in aquaculture. In our work, a quick screening approach was developed for the qualitative and semi-quantitative screening of 87 pesticide residues in aquatic products. The sample preparation was investigated, including extract solvent, extract methods, buffer salts, lipid removal, cleanup materials and filter membranes for aquatic products. Samples were extracted using a modified QuEChERS procedure, and two clean-up procedures were developed for UHPLC-Q/Orbitrap MS analysis based on the fat content of the aquatic products. The screening detection limits for all studied pesticides were distributed between 1 and 500 μg/kg in the three representative matrices. Seventy-one pesticides could be analyzed with a screening limit between 1 and 25 μg/kg in grass carp and crayfish, sixty-one pesticides could be screened for limits between 1 and 50 μg/kg in crab. The accuracy results showed that recoveries ranged from 50 to 120% for 60, 56 and 52 pesticides at medium-level for grass carp, crayfish and crab, respectively. At high spiking levels, 74, 65 and 59 pesticides were recovered within the range of 50–120% for the three matrices, respectively. The relative standard deviations of most compounds in different matrices were less than 20%. With this method, the local farmed aquatic products were tested for pesticide residues. In these samples, ethoxyquinoline, prometryn and phoxim were frequently detected. The majority of these confirmed compounds did not exceed 2.00 μg/kg. A grass carp with trichlorfon at 4.87 μg/kg and two carps with ethoxyquinoline at 200 µg/kg were detected, indicating the potential dietary risk.

Edible chrysanthemum is widely cultivated and used as an important ingredient of medicine, tea and multifunctional food. During the planting of chrysanthemum, pesticides are extensively used for preventing plant diseases and insect pests. To ensure the food safety of edible chrysanthemum, rapid detection methods are urgently needed for on-site inspection. In this study, a graphene oxide/Au nanoparticle (GO/Au NP) cellulose substrate was prepared through layer-by-layer assembly of GO and Au NPs on a mixed cellulose ester membrane. Surface-enhanced Raman spectroscopy (SERS) detection of four types of organophosphorus and organosulfur pesticides was achieved by filtering the extracting solution through the substrate and analysing SERS spectra. Qualitative and semi-quantitative detection of fenthion, phoxim, isocarbophos and thiram was accomplished with the detection limits of 38.01, 8.13, 48.97 and 8.74 ng mL⁻¹, respectively. A spiking experiment further demonstrated the feasibility of this method for rapid and on-site detection of mixed pesticides in chrysanthemum. This study provides a new approach for rapid detection of multiple hazardous substances in flowering and herbal plants.