Benzoylurea Pesticides Research Articles

Polyamidoamine dendrimer-functionalized silica nanocomposite with polydopamine coating for dispersive micro solid-phase extraction of benzoylurea insecticides in water samples

近年来,由农药残留导致的环境污染问题已引起社会的广泛关注,开发便捷高效的分析方法对农药残留进行检测和监测十分必要。研究设计并成功制备了聚多巴胺涂敷的聚酰胺-胺树状分子功能化的二氧化硅复合材料(SiO2-PAMAM-PDA),并采用透射电镜对其进行表征。开发了以此复合材料为吸附剂的分散微固相萃取方法(D-μ-SPE),并结合高效液相色谱对水基质中的4种苯甲酰脲类杀虫剂(BUs)残留进行了富集检测。多巴胺结构中含有丰富的苯环、氨基及羟基,可与目标物形成氢键、π-π相互作用,从而增强了材料对苯甲酰脲的萃取能力。对吸附剂用量、萃取时间等可能影响萃取效率的条件进行了单因素优化。在最优条件下,该方法的线性范围在10~500 μg/L之间,根据3倍信噪比(S/N)计算所得的检出限(LOD)为1.1~2.1 μg/L,回收率为82.8%~94.1%,相对标准偏差(RSD)为2.1%~8.0%。将建立的方法与已报道的以苯甲酰脲作为目标物的方法进行了对比,发现方法样品用量及萃取剂用量均较少,且所需前处理时间较短,有机溶剂消耗也较少,为苯甲酰脲类农药的检测提供了更快速、绿色的选择。为评估所开发方法的实际样品适用性,将其应用于3种河水样品中4种苯甲酰脲类杀虫剂的分析检测,所得回收率及RSD分别为69.5%~99.4%和0.2%~9.5%,表明此方法在实际样品中同样具有较高的准确性和精密度。

Ameliorative effect of avocado oil against lufenuron induced testicular damage and infertility in male rats.

Lufenuron is a benzoylurea pesticide that causes significant histological and histochemical damage in mammals. Avocado is a common food in the human diet that contains antioxidant and antitumor properties. In male rats, avocado oil's protection against lufenuron-induced reproductive deterioration, oxidative stress, and DNA damages was investigated. Twenty-eight mature male rats were selected and distributed into four groups: Group 1, control group were administered distilled water orally; Group 2 received 4ml/kg avocado; Group 3 was given lufenuron (1.6mg/kg), and Group 4 was given avocado oil/lufenuron. The findings show that lufenuron treatment reduces reproductive hormone levels, sperm count, motility, viability and causes negative histopathological changes in testicular tissue, such as decreased epithelial height and increased luminal diameter degenerated spermatogenesis. Furthermore, lufenuron reduced the content of antioxidant enzymes while increasing the level of malondialdehyde, nitric oxide and corresponding DNA damage. Results showed that lufenuron is associated with testicular function impairment, which leads to infertility. Treatment with avocado oil improved reproductive hormone secretions, enzymatic activity, histological and DNA damage parameters in testis tissues, reducing the negative effects of lufenuron, proving that it may have a therapeutic role against lufenuron-mediated testicular toxicity.

A monolithic capsule phase microextraction method combined with HPLC-DAD for the monitoring of benzoyl urea insecticides in apple juice samples

Fruit juices may contain harmful residues of pesticides that are associated with ecological and health risks. Thus, it is critical to develop sensitive and accurate methods for the monitoring of pesticides in these food products. In the present study, a simple and sensitive capsule phase microextraction (CPME) protocol combined with high-performance liquid chromatography-diode array detection (HPLC-DAD) was developed for the monitoring of benzoyl urea pesticides (chlorfluazuron, diflubenzuron, hexaflumuron, lufenuron, and triflumuron) in apple juices. Among the different examined sorptive phases, monolithic sol–gel poly(caprolactone)-poly(dimethylsiloxane)-poly(caprolactone) capsules were found to exhibit the highest extraction efficiency. The adsorption and desorption steps of the CPME method were optimized and the proposed method was validated. Under optimum conditions, the limits of detection for all analytes were in the range 0.15–0.30 ng mL−1. Moreover, the proposed protocol exhibited good linearity, accuracy, and precision. The relative recoveries of the method ranged between 90% and 108%, and the relative standard deviations were <8% and 9% for intra-day and inter-day precision, respectively. The ComplexGAPI index was used to evaluate the green potential of the proposed method. Finally, the proposed method was employed in the analysis of a wide variety of commercially available apple juice samples.

TiO2@MOF-919(Fe-Cu) as a sorbent for the extraction of benzoylurea pesticides from irrigation water and fruit juices.

The TiO2@MOF-919(Fe-Cu) solid-phase extraction material was prepared by growing MOF-919(Fe-Cu) in situ on three-dimensional radial TiO2 microspheres by a simple solvothermal method. This combination drew on both the resources of good single dispersion and extraction rate, which made it a better extraction material. It was accompanied with high-performance liquid chromatography (SPE-HPLC) for the separation and determination of four benzoylurea pesticides (triflumuron, chlorbenzuron, teflubenzuron and diflubenzuron) in afforestation irrigation water and juice samples (grape, peach and apple juices). Under the optimal conditions, the linearity of the method ranged from 1 to 400 μg L-1 with a correlation coefficient (R2) ≥ 0.9994, while the detection limit was in the range of 0.40-0.56 μg L-1 for the four pesticides. The adopted material showed good reusability and can be used no less than 10 times. The intra-day and inter-day precision were in the range of 1.78-3.24% and 4.06-5.08%, respectively. The proposed method was then successfully applied for the detection of benzoylurea pesticides in the spiked samples with good recoveries (72.3-108.4%) and good precision (5.15%) due to π-π and hydrophobic interactions between the analytes and adsorbent. The results show that the composite had the potential to be used as a SPE adsorbent for the enrichment and extraction of benzene ring structures containing imide groups in actual samples.

Phenylboronic acid-functionalized cross-linked chitosan magnetic adsorbents for the magnetic solid-phase extraction of benzoylurea pesticides.

In this study, a 4-formylphenylboronic acid-modified cross-linked chitosan magnetic nanoparticle (FPBA@CCHS@Fe3 O4 ) was fabricated. The synthesized material was utilized as the magnetic solid-phase extraction adsorbent for the enrichment of six benzoylurea pesticides. In addition to B-N coordination, FPBA@CCHS@Fe3 O4 interacts with benzoylureas through hydrogen bonds and π-π stacking interaction on account of rich active groups (amino and hydroxyl) and aromatic rings in structure. Compared to traditional extraction methods, less adsorbent (20mg) and reduced extraction time (3min) were achieved. The adsorbent also exhibited good reusability (no less than 10 times). Coupled with a high-performance liquid chromatography-diode array detector, satisfactory recoveries (89.1-103.9%) and an acceptable limit of detection (0.2-0.7 μg/L) were obtained. Under optimized conditions, the established method was successfully applied to the tea infusion samples from six major tea categories with acceptable recoveries ranging from 76.8 to 110%, indicating its application potential for the quantitative detection of pesticides in complex matrices.

Photo-degradation behavior of seven benzoylurea pesticides with C3N4 nanofilm and its aquatic impacts on Scendesmus obliquus

Present concerns on the residual benzoylurea pesticides (BUPs) are rapidly climbing as their market shares increase and now seven typical compounds were picked to study their photo-degradation behavior and ecological impacts. Carbon nitride (C3N4) nanofilm at a thickness of 50–80 nm was built on the glass slides and utilized to evaluate the photostability of pesticides under visible light. The results showed that the nano-C3N4 can promote the degradation efficiency of BUPs and it follows the first-order dynamic mechanism. They could be divided into three categories with the substituents and their degradations were discriminated in order of chlorofluoro-, chlorofluoroalkoxy- and chlorofluorophenoxy- substituted ones. Analyzing the intermediates by UHPLC-MS, it can be speculated that the similar pathways came to BUPs such as cleavage of urea-bridge, hydroxylation and dehalogenation. It is attractive that they all passed into a same molecule, 2-fluorobenzamide (m/z, 301.14). Moreover Scendesmus obliquus was applied to indicate the ecological impacts of originals and their photoproducts. Exposed to pesticides, the levels of chlorophyll a demonstrated much more inhibition than chlorophyll b. Lufenuron and chlorfuazuron among seven showed the higher toxicity for algal cells and finally the photodegradation products showed the lowest toxicity. The activities of antioxidant enzymes happened to a significant remedy after photodegradation. It can be concluded that the residual BUPs under visible-light irradiation may degrade through similar pathways and reduce the aquatic toxicity with the presence of C3N4 nanofilm.

Diflubenzuron leads to apoptotic cell death through ROS generation and mitochondrial dysfunction in bovine mammary epithelial cells

Pesticides, which are used in agriculture and forestry to eliminate insects, are a major cause of environmental pollution. Among them, diflubenzuron (DFB), 1-(4-chlorophenyl)-3-(2,6-difluorobenzoyl) urea, is a common benzoylurea insecticide that hinders larval development, primarily in Aedes aegypti larvae. Many experts have announced the biological toxicity of DFB in various species. However, the toxicity of benzoylurea pesticides, including DFB, to bovine mammary epithelial cells (MAC-T) is unclear. Therefore, in this study, we confirmed the cytotoxic effects of DFB on the viability and proliferation of MAC-T cells. Additionally, we observed that DFB induced lipid peroxidation through reactive oxygen species (ROS) production, resulting in an increase in transcriptional gene expression related to inflammatory response. Moreover, we demonstrated mitochondrial dysfunction including depolarization of the mitochondrial membrane, perturbation of calcium homeostasis, and, eventually, apoptosis. Furthermore, we identified DFB-triggered signaling pathways related to ROS generation and cell proliferation, as well as their interactions, by treating the cells with pharmacological inhibitors in combination with DFB. DFB attenuated the phosphorylation of AKT, P70S6K, S6, and ERK1/2 and facilitated the phosphorylation of JNK and c-Jun. These results show that DFB can induce apoptotic cell death via ROS generation and mitochondrial dysfunction in MAC-T cells.

Flufenoxuron suppresses the proliferation of testicular cells by targeting mitochondria in mice

Flufenoxuron is a benzoylurea pesticide that is used to eradicate insects and acarids in the farmland. Even though it specifically works on target animals, the possibilities of its bioaccumulation and harmful effects on non-target animals cannot be denied. As the usage and application of pesticides increases, exposure to them also increases through ingestion of food residues, inhalation, or dermal contact. Pesticides could also be considered as endocrine disruptor chemicals; however, the reproductive toxicity and cellular mechanisms of flufenoxuron have not been identified. Our results indicate that flufenoxuron inhibits cellular proliferation and hampers calcium homeostasis, especially by targeting mitochondria. We also confirmed the induction of endoplasmic reticulum (ER) stress and ER-mitochondrial contact signaling. Using pharmacological inhibitors, we also observed that the mitogen-activated protein kinase and Akt signaling pathways were upregulated by flufenoxuron. Further, by oral administration of flufenoxuron (100 mg/kg/bw) to C57BL/6 male mice, we observed transcriptional changes in the testis-related genes. Collectively, we demonstrated that flufenoxuron inhibits cell proliferation and alters gene expression in mouse testis cells and induces testicular dysfunction in mice. These results indicate that flufenoxuron may be harmful to male reproduction and fertility in the early stages of pregnancy.

PEG-modified magnetic Schiff base network-1 materials for the magnetic solid phase extraction of benzoylurea pesticides from environmental water samples

It is necessary to establish a rapid, simple and environmentally friendly detection method for benzoylurea pesticides (BUs) in environmental water samples because of their toxicity in environmental circulation. Herein, a novel polyethylene glycol (PEG) modified magnetic covalent organic framework material based on the Schiff base reaction was prepared (PEG/Fe3O4@SNW-1). This material was used as a sorbent for enriching five BUs by magnetic solid phase extraction prior to detection via high-performance liquid chromatography. After the optimization of several parameters (such as the salinity, extraction time, amount of sorbent, desorption time, etc.) that influenced the recovery of the magnetic solid phase extraction process, the limits of detection (S/N = 3) were defined as less than 1.0 μg L−1, and the limits of quantitation (S/N = 10) were calculated as being lower than 3.4 μg L−1. A satisfactory linear range of 5–1000 μg L−1 was achieved. Finally, the proposed method was applied to analyze benzoylurea pesticides in three environmental water samples. These results indicated that the proposed method was feasible and demonstrated the potential application of the PEG/Fe3O4@SNW-1 material for detecting similar pesticide residues in environmental water samples.

Extraction of benzoylurea pesticides from tea and fruit juices using deep eutectic solvents

In this study, low-density deep eutectic solvent combined with dispersive liquid-liquid microextraction was applied to the extraction of five benzoylurea insecticides (BUs, including diflubenzuron, triflumuron, hexaflumuron, flufenoxuron, and chlorfluazuron) from beverages. Then the extracted and concentrated samples were analyzed and detected using the high-performance liquid chromatography combined with an ultraviolet detector. The DESs were synthesized by [P14,6,6,6]Cl as hydrogen bond acceptor and tetradecyl alcohol as hydrogen bond donor, and then characterized by Fourier transform infrared spectroscopy. In the experiment, the key factors affecting the extraction efficiency were screened by Plackett-Burman design and optimized with the central composite design. The extraction recovery rates were 85.91–95.12%. The limits of detection and correlation coefficients of the method were 0.30–0.60 μg L−1 and 0.9992–0.9997. Finally, the method was applied to determine the BUs in four beverage samples, and satisfactory recoveries, within the range of 76.87–101.19% were achieved. The present method has the potential to be applied to the detection of BUs in aqueous samples.

Simultaneous determination of carbamate and benzoylurea pesticides in vegetables and fruits with QuEChERS method

Simultaneous determination of carbamate and benzoylurea pesticides in vegetables and fruits with QuEChERS method

Acetylcholinesterase of mangrove oyster Crassostrea rhizophorae: A highly thermostable enzyme with promising features for estuarine biomonitoring

Enzyme biomarkers from several aquatic organisms have been used for assessing the exposure to contaminants at sublethal levels. Amongst them, the cholinesterases are commonly extracted from several organisms to evaluate/measure organophosphate and carbamate neurotoxic effects. Acetylcholinesterase (AChE; EC 3.1.1.7) is an enzyme of the group of serine esterases that acts on the hydrolysis of the neurotransmitter acetylcholine allowing the intermittence of the nerve impulses responsible for the neuronal communication. This enzyme is the main target for the action of some pesticides and the inhibition of its activity in bivalve mollusks may be used as biomarker due to their filter-feeding habit. In this context, the present study aimed to characterize physicochemical and kinetic parameters of the AChE extracted from gills and viscera of the oyster Crassostrea rhizophorae and investigate the in vitro effect of pesticides (dichlorvos, diazinon, chlorpyrifos, methyl-parathion, temephos, carbaryl, carbofuran, aldicarb, diflubenzuron and novaluron) in search for assessing its potential as biomarker. Specific substrates and inhibitors evidenced the predominance of AChE in both tissues. The optimum pH found for gills and viscera AChE were 8.0 and 8.5, respectively. The maximum peak of activity occurred at 70 °C for gill AChE and 75 °C for viscera AChE. The enzymes of both tissues presented remarkable thermostability. The Michaelis-Menten constant for both enzymes were 1.32 ± 0.20 mM for gills and 0.43 ± 0.12 mM for viscera. The Vmax values for gills and viscera were 53.57 ± 1.72 and 27.71 ± 1.15 mU/mg, respectively. The enzymes were able to reduce the activation energy to 9.75 kcal mol−1 (gills) and 11.87 kcal mol−1 (viscera) obtaining rate enhancements of 3.57 × 105 and 1.01 × 104, respectively, in relation to non-catalyzed reactions. Among the pesticides under study, the carbamates carbaryl and carbofuran exerted the strongest inhibitory effects on the enzyme activity achieving important degrees of inhibition at concentrations below national and international current regulations. The first observation of the effects of benzoylurea pesticides (diflubenzuron and novaluron) on AChE from mollusks is reported here. The gills AChE of C. rhizophorae showed potential to be specific biomarker for the carbamate carbaryl while the viscera AChE showed it for carbofuran. According to their features, these enzymes may be proposed as promising tools for estuarine monitoring as well as biocomponent of biosensor devices.

The tissue distribution, metabolism and hepatotoxicity of benzoylurea pesticides in male Eremias argus after a single oral administration

Benzoylurea pesticides (BPUs) are widely used to control the locust, but the toxicokinetics and hepatotoxicity of BPUs in lizards have not been investigated. In this study, the tissue distribution, metabolism and liver toxicity of diflubenzuron and flufenoxuron were assessed in the Eremias argus following a single oral exposure. Diflubenzuron preferred to accumulate in the fat and brain (>1.0 mg kg−1) and was rapidly eliminate in other tissues. In the liver, 4-chloroaniline was one of diflubenzuron metabolites, although with a concentration less than 0.05% of the accumulated diflubenzuron. No significant difference was observed in the liver histopathology between the control and diflubenzuron exposure group. The expressions of Cyp1a and Ahr gene which control the cell apoptosis were also equal to the control level. After flufenoxuron exposure, biomodal phenomenon was observed in the liver, skin, brain, gonad, kidney, heart and blood circulation was an important route for the flufenoxuron penetration. The concentrations of flufenoxuron in all tissues were greater than 1.0 mg kg−1 at 168 h. The excretion of flufenoxuron in the faeces was 1.5 fold higher than diflubenzuron. The hepatocytes in the flufenoxuron treated group showed vacuolation of cytoplasm and decreased nucleus. In addition, the Cyp1a and Ahr genes were significantly up-regulated in the flufenoxuron exposure group. These results suggested that the higher hepatotoxicity of flufenoxuron may be attributed to the higher residual level in the lizard tissues and the Cyp1a and Ahr genes can serve as biomarkers to assess the liver toxicity.

Acute and chronic toxicity of the benzoylurea pesticide, lufenuron, in the fish, Colossoma macropomum

Lufenuron is a benzoylurea insecticide that interfere in chitin synthesis in insects. Although lufenuron is widely used in agriculture and aquaculture, rare are studies described that relates to possible toxic effects in fish. This work aimed to evaluate acute and chronic toxic effects of benzoylurea pesticide (lufenuron) on biological parameters of Colossoma macropomum (Tambaqui). In the acute test, juveniles of Tambaqui were divided into control group and five experimental groups with exposure from 0.1 to 0.9 mg/L of lufenuron for 96 h. Animals were also submitted to chronic toxicity test for four months in concentrations of 0.1 and 0.3 mg/L of lufenuron, the concentration used in the treatment of ectoparasites in fish and 50% of LC50 96 h, respectively. The presence of hemorrhages was observed in eyes, fins and operculum of fish exposed to 0.7 and 0.9 mg/L of lufenuron. Histological analysis showed changes in the morphology of fish gills submitted to acute toxicity test, as lamellar aneurysm and blood congestion inside lamellae. Lufenuron promoted damage in fish retina as in ability to respond to stimuli in photoreceptors and in ON-bipolar cells in acute test. In chronic test, blood glucose analysis and morphometric parameters showed no significant differences (p > 0.05). In general, Tambaqui exhibited behaviors associated with stress when exposed to lufenuron. Thus, lufenuron showed several toxic effects in relation to biological parameters in Tambaqui. This concerns about the use and discard of lufenuron, and indicates the requirement of environmental actions to prevent potential contamination of aquatic biota.

Benzoylurea pesticides used as veterinary medicines in aquaculture: Risks and developmental effects on nontarget crustaceans.

Diflubenzuron and teflubenzuron are benzoylureas that are used in aquaculture to control sea lice. Flubenzurons have low toxicity to many marine species such as fish and algae but by their nature are likely to have significant adverse effects on nontarget species such as crustaceans and amphipods. Although the exact mechanism of toxicity is not known, these compounds are thought to inhibit the production of the enzyme chitin synthase during molting of immature stages of arthropods. These chitin synthesis inhibitors are effective against the larval and pre-adult life stages of sea lice. Due to their low solubility and results of recent monitoring studies conducted in Norway, the sediment compartment is considered the most likely reservoir for these compounds and possible remobilization from the sediment to benthic crustaceans could be of importance. For this reason, the epibenthic copepod Tisbe battagliai was selected for investigations into the acute and developmental effects of these compounds. For comparative purposes, azamethiphos was investigated to identify differences in sensitivity and act as a negative control for developmental effects at environmentally relevant concentrations. Standard acute studies with adult copepods showed little or no acute toxicity at milligrams per liter levels with the flubenzurons, whereas a naupliar developmental test demonstrated that environmentally relevant concentrations (e.g., nanograms per liter) caused a complete cessation of molting and finally death in the exposed copepods.

Unique Graphitic Carbon Nitride Nanovessels as Recyclable Adsorbent for Solid Phase Extraction of Benzoylurea Pesticides in Juices Samples

Unique graphitic carbon nitride (g-C3N4) nanovessels have been prepared and applied as solid phase extraction (SPE) adsorbent for determining benzoylurea pesticides (BUs) in different juice samples using high performance liquid chromatography (HPLC) equipped with ultraviolet detection (UVD). The g-C3N4 nanovessels were obtained on a large scale by thermally converting low-cost urea without additive assistance, which avoided a complex synthesis process, consumption of organic solvent, and limits of tailoring the reaction pressure and atmosphere. The g-C3N4 nanovessels have been characterized using transmission electron microscope (TEM), Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET) analysis, and elemental analysis. The conditions affecting the extraction efficiency were optimized, including adsorbent amount, extraction time, sample volume, and choice and volume of desorption solvent. Under the optimal conditions, comparable detection limits of 6 μg/L and good recoveries of 70.4–96.4 % for six BUs have been achieved. Meanwhile, g-C3N4 nanovessels showed excellent reuse potential for ten times. The results indicated that g-C3N4 nanovessels repesented a promising SPE adsorbent for the enrichment and trace analysis of pollutants.

Crystal structure of flufenoxuron: a benzoyl-urea pesticide.

The title compound, C21H11ClF6N2O3 (systematic name: 1-{4-[2-chloro-4-(trifluoromethyl)phenoxy]-2-fluorophenyl}-3-(2,6-di­fluoro­benzo­yl)urea), is a benzoyl­urea pesticide. The dihedral angles between the central fluoro­benzene ring and the terminal di­fluoro­phenyl ring and chloro­phenyl ring system are 62.15 (5) and 88.03 (5)°, respectively. In the crystal, N—H⋯O hydrogen bonds link adjacent mol­ecules, forming R 2 2(8) inversion dimers that pack into loop chains along the a-axis direction by short F⋯F contacts [2.729 (2) Å]. In addition, the chains are linked by weak C—H⋯π and π–π inter­actions [inter-centroid distances = 3.661 (2) and 3.535 (12) Å], resulting in a three-dimensional architecture.

[Preparation of boronate affinity sorbent and its extraction performance for benzoylurea pesticides]

A new boronate affinity monolithic material was prepared and used as the extraction medium of stir cake sorptive extraction (SCSE). The porous boronate affinity sorbent was prepared by in situ copolymerization of 3-acrylamidophenylboronic acid (APB) and divinyl benzene (DVB). To achieve optimum extraction performance for benzoylurea pesticides, several parameters, including desorption solvent, pH value, ionic strength in sample matrix, extraction and desorption times, were investigated in detail. At the same time, a simple, sensitive and environment friendly method for the determination of benzoylurea pesticides in water and juice samples was developed by the combination of SCSE-APBDVB with HPLC equipped with a diode array detector. Under the optimized experimental conditions, the limits of detection (S/N = 3) for target analytes were 0.055-0.11 μg/L in water and 0.095-0.31 μg/L in juice. The precision of the proposed method was evaluated in terms of intra- and inter-assay repeatability calculated as RSD, and it was found that the RSDs were all below 9.0%. The developed method was successfully applied to the determination of benzoylurea pesticide residues in water and juice samples and satisfactory recoveries of spiked target compounds were in the range of 75.6%-109%. The results well demonstrate that the new sorbent can extract benzoylurea pesticides effectively through multi-interactions including boron-nitrogen coordination, hydrogen-bond and hydrophobic interactions between sorbent and analytes.

Study on the simultaneous determination of seven benzoylurea pesticides in Oolong tea and their leaching characteristics during infusing process by HPLC–MS/MS

A method for the simultaneous determination of 7 benzoylurea pesticides (chlorfluazuron, diflubenzuron, fluazuron, flufenoxuron, hexaflumuron, teflubenzuron and triflumuron) in the manufactured Oolong tea leaves and its infusion was described. The method has a LOD of 0.03–1.00ng/mL, a recovery of 90.4–103% for made tea and 90.3–102% for tea-infused liquid, respectively. By using the proposed method, the leaching characteristics of above 7 pesticides during infusing process were investigated. The experimental results revealed that: (1) diflubenzuron can be most easily extracted out during infusing process, followed by triflumuron, teflubenzuron, hexaflumuron, chlorfluazuron, flufenoxuron and fluazuron. (2) The leaching of flufenoxuron and chlorfluazuron during infusing process seems to be controlled by only their solubility, whereas, the leaching of other 5 benzoylurea insecticides was primarily controlled by their partitioning coefficient between made tea and hot water. The results of this study are helpful for the accurate evaluation of the safety of Oolong tea.

Dispersive liquid-phase microextraction in combination with HPLC for the enrichment and rapid determination of benzoylurea pesticides in environmental water samples

Benzoylurea (BU) insecticides have contributed greatly to the output of crops. Their residue in the environment put serious threats on human health and environmental safety. In this study, we have established a new, rapid, and reliable method for the monitoring of typical BU insecticides such as diflubenzuron, flufenoxuron, triflumuron, and chlorfluazuron with dispersive liquid-liquid microextraction prior to HPLC. Chlorobenzene and ethanol were employed as the extraction solvent and disperser solvent, respectively. The possible parameters which would influence the extraction efficiency such as the kinds and volumes of extraction and disperser solvents, extraction time, sample pH, centrifuging time, and salting-out effect were optimized in detail. Under the optimal conditions, the linear range of proposed method was in the range of 1.0-70 μg/L. The detection limits varied from 0.24 to 0.82 μg/L and the precision of the method was <6.5% (RSD, n = 6). The proposed method was validated with real water samples and satisfactory spiked recoveries were achieved. All these results indicate that the proposed method is a low cost, easy to operate, efficient, and sensitive method for the analysis of BU insecticides in water samples.