Huizhen Wu

Variations in the fate and biological effects of sulfamethoxazole, norfloxacin and doxycycline in different vegetable-soil systems following manure application.

The fate of sulfamethoxazole (SMZ), norfloxacin (NOR) and doxycycline (DOX) and their biological effects in radish and pakchoi culture systems were investigated. DOX dissipated more rapidly than SMZ and NOR, while radish and pakchoi cultivation increased the removal of residual DOX in soils. Dissipation of NOR was accelerated in radish soils but was slowed down slightly in pakchoi soils. Vegetable cultivation exerted an insignificant effect on SMZ removal. Investigation of antibiotic bioaccumulation showed that the uptake of DOX by radish and pakchoi was undetectable, but the radish accumulated more SMZ and NOR than pakchoi. Among the three antibiotics, only SMZ use exhibited an apparent suspension of plant seed germination, up-ground plant growth and soil microbial diversity. Pakchoi responded more sensitively to SMZ than did the radish. Principal component analysis (PCA) based on MicroRESP™ indicated that the sampling time and antibiotic treatments could influence the soil microbial community. Only in the pakchoi soils did antibiotic application exert a more robust effect on the microbial community than the sampling time; SMZ treatments and DOX treatments could be clearly discriminated from the control treatments. These results are crucial for an assessment of the potential risks of antibiotics to culture system practices and suggest that good agricultural practices help to limit or even reduce antibiotic pollution.

Occurrence of trace elements and antibiotics in manure-based fertilizers from the Zhejiang Province of China

The occurrence of seven trace elements and forty three antibiotics was investigated in manure-based fertilizers from the Zhejiang province of China. These trace elements included copper, zinc, arsenic, chromium, mercury, lead and cadmium. The targeted antibiotics included four groups: sulfonamides, tetracyclines, fluoroquinolones and chloramphenicols. The median amounts of copper, zinc, arsenic, chromium, mercury, lead and cadmium in the analyzed samples were 160, 465, 7.9, 21.2, 0.3, 8.1 and 0.6mg·kg(-1), respectively. Seventeen antibiotics were detected. Enrofloxacin was the most frequently detected compound, with a detection rate of 39.3% and concentrations ranging from 6.7μg·kg(-1) to 4091μg·kg(-1). Based on the referred loading rates in agricultural soil, 10% of the collected manure-based fertilizer samples might pose a high potential ecological risk due to the presence of antibiotics.

Ultrasound/microwave-assisted solid–liquid–solid dispersive extraction with high-performance liquid chromatography coupled to tandem mass spectrometry for the determination of neonicotinoid insecticides in Dendrobium officinale

A one-step ultrasound/microwave-assisted solid-liquid-solid dispersive extraction procedure was used for the simultaneous determination of eight neonicotinoids (dinotefuran, nitenpyram, thiamethoxam, clothianidin, imidacloprid, acetamiprid, thiacloprid, imidaclothiz) in dried Dendrobium officinale by liquid chromatography combined with electrospray ionization triple quadrupole tandem mass spectrometry in multiple reaction monitoring mode. The samples were quickly extracted by acetonitrile and cleaned up by the mixed dispersing sorbents including primary secondary amine, C18 , and carbon-GCB. Parameters that could influence the ultrasound/microwave-assisted extraction efficiency such as microwave irradiation power, ultrasound irradiation power, temperature, and solvent were investigated. Recovery studies were performing well (70.4-113.7%) at three examined spiking levels (10, 50, and 100 μg/kg). Meanwhile, the limits of quantification for the neonicotinoids ranged from 0.87 to 1.92 μg/kg. The method showed good linearity in the concentration range of 1-100 μg/L with correlation coefficients >0.99. This quick and useful analytical method could provide a basis for monitoring neonicotinoid insecticide residues in herbs.

Magnetic dispersive solid-phase extraction based on a novel adsorbent for the detection of triazole pesticide residues in honey by HPLC-MS/MS

A novel Fe3O4@MDN magnetic nanomaterial was successfully developed as a magnetic dispersive solid-phase extraction adsorbent for the determination of triazole pesticide residuals in honey samples by high performance liquid chromatography coupled with triple quadrupole mass spectrometry (HPLC-MS/MS). The macromolecular structure named MDN was coated on the surface of a copolymer synthesized with silyl reagents methacrylic acid-3-(trimethoxysilyl) propyl ester (MPS) and tetraethyl orthosilicate (TEOS) based on ferriferrous oxide (Fe3O4), whose characteristics were confirmed by a scanning electron microscope (SEM). The proposed magnetic dispersive solid-phase extraction (MDSPE) method provided a rapid, environmentally friendly and magnetic stuff recyclable approach for the triazole pesticide analysis. By means of optimal conditions, the recoveries of 15 triazoles (spiked at 20 μg kg−1) ranged from 90.5 to 105.9%. The method showed good linearity, sensitivity in the range of μg per kilogram and repeatability (relative standard deviation below 6.8%, n = 5). The proposed method was confirmed to be a simple, rapid and efficient method for the analysis of triazole pesticide residuals in honey samples.

Simultaneous determination of florfenicol with its metabolite based on modified quick, easy, cheap, effective, rugged, and safe sample pretreatment and evaluation of their degradation behavior in agricultural soils

A simple and simultaneous method for the determination of florfenicol and its metabolite florfenicol amine in agricultural soils using modified quick, easy, cheap, effective, rugged, and safe sample pretreatment and reversed-phase high-performance liquid chromatography with tandem mass spectrometry is presented. Florfenicol and its metabolite florfenicol amine residues in agricultural soils were extracted with alkalized acetonitrile and an aliquot was cleaned up with Si(CH2)3NH(CH2)2NH2 and C18 sorbent, which were powder materials. High-performance liquid chromatography with tandem mass spectrometry was applied to simultaneously determine the level of florfenicol and florfenicol amine in agricultural soils. Excellent linearity was achieved for florfenicol and florfenicol amine over a range of concentrations from 0.1-500 μg/L with coefficients more than 0.99. Average recoveries at four different levels (0.005, 0.05, 0.5, and 5.0 mg/kg) for florfenicol and florfenicol amine ranged from 73.6-94.9% with relative standard deviations of 2.9-12.5%. The limits of detection for florfenicol and florfenicol amine in agricultural soils were 2.0 μg/kg, and the limits of quantification were 6.0 μg/kg. Based on this method, the degradation behavior of florfenicol and its metabolite florfenicol amine in three soils (Nanchang, Hangzhou, and Changchun) under sterilized and native conditions was investigated and the transformation rate of florfenicol amine from florfenicol was evaluated.

Development and application of an in-cell cleanup pressurized liquid extraction with ultra-high-performance liquid chromatography-tandem mass spectrometry to detect prohibited antiviral agents sensitively in livestock and poultry feces

An in-cell cleanup pressurized liquid extraction was developed to analyze prohibited antiviral agents in livestock and poultry feces. Extraction and cleanup were integrated into one step. The extraction was performed using methanol-acetonitrile (1:1, v/v) with 0.5% glacial acetic acid at 90°C, and 0.75g of PSA was used as the adsorbent during the extraction procedure. Under optimal conditions, the average recoveries for 11 antiviral drugs were 71.5-112.5% at three spiked levels (20, 40, and 100μgkg-1). The detection limits and detection quantitations of the analysis method for the eleven antiviral drugs were 0.6-1.4 and 1.4-4.7μgkg-1, respectively. Finally, the method was applied to analyze amantadine, oseltamivir and its metabolites oseltamivir acid in duck feces based on an experiment of an oral dose of two antiviral drugs in duck. The amantadine, oseltamivir and oseltamivir acid can be detected in feces within approximately four weeks after amantadine and oseltamivir were orally administered. The results indicate that the residue analysis in feces is a noninvasive method to monitor inhibited antiviral agents efficiently in livestock and poultry breeding.

Determination of Pyrethroids in Dendrobium officinale by Ultrasound/Microwave-Assisted Solid–Liquid–Solid Dispersive Extraction, Gas Chromatography, and Triple-Quadrupole Mass Spectrometry

ABSTRACT An ultrasound/microwave-assisted solid–liquid–solid dispersive extraction method was developed for the determination of 16 pyrethroid insecticides in Dendrobium officinale. The extraction and purification were performed in one step. The pyrethroids were extracted with 8:2 acetone:hexane and purified with a mixture of primary secondary amine, Florisil, C18, and graphitized carbon black. The extraction temperature, extraction time, and ultrasound power were optimized. Trans-cyfluthrin-d6 was used as the internal standard to improve the accuracy. Under the optimized conditions, the recoveries of the pyrethroids were from 72.2 to 113.9% with the limits of detection between 0.29 and 9.38 µg kg−1. The optimized method was successfully used for the determination of pyrethroids in commercial D. officinale samples and may allow monitoring pyrethroids in herbal products.