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1.
J Agric Food Chem ; 72(12): 6613-6624, 2024 Mar 27.
Artigo em Inglês | MEDLINE | ID: mdl-38501445

RESUMO

Propaquizafop is a highly efficient aryloxy phenoxy propionate chiral herbicide. However, the use of propaquizafop, including its safe use methods, residue patterns, dietary risk assessment, and maximum residue limits, for ginseng, a traditional Chinese medicinal plant, has not been studied. An analytical method was established for the simultaneous determination of propaquizafop and its four metabolites in ginseng soil, fresh ginseng, ginseng plant, and dried ginseng using HPLC-MS/MS. This approach showed good linearity (R2 ranging from 0.9827 to 0.9999) and limit of quantification ranging from 0.01 to 0.05 mg/kg. The intra- and interday recovery rates of this method ranged from 71.6 to 107.1% with relative standard deviation ranging from 1.3 to 23.2%. The method was applied to detect residual samples in the field, and it was found that the degradation of propaquizafop in ginseng plants and soil followed a first-order kinetic equation. R2 was between 0.8913 and 0.9666, and the half-life (t1/2) ranged from 5.04 to 8.05 days, indicating that it was an easily degradable pesticide (T1/2 < 30 days). The final propaquizafop residues in ginseng soil, plants, fresh ginseng, and dried ginseng ranged from 0.017 to 0.691 mg/kg. A dietary risk assessment was conducted on the final propaquizafop residue in fresh and dried ginseng. The results showed that the chronic exposure risk quotient values were less than 100% for fresh and dried ginseng (1.15% for fresh ginseng and 1.13% for dried ginseng). This illustrates that the dietary risk associated with the use of 10% propaquizafop emulsifiable concentrate in ginseng is very low. Thus, applying 750 mL/ha of propaquizafop on ginseng could not pose an unacceptable risk to public health. The results of the present study support the registration of propaquizafop in ginseng.


Assuntos
Panax , Resíduos de Praguicidas , Poluentes do Solo , Espectrometria de Massas em Tandem/métodos , Panax/química , Resíduos de Praguicidas/análise , Poluentes do Solo/química , Medição de Risco , Meia-Vida , Solo/química , China
2.
Ecotoxicol Environ Saf ; 274: 116199, 2024 Apr 01.
Artigo em Inglês | MEDLINE | ID: mdl-38492485

RESUMO

This study established a residue detection method based on the QuEChERS pre-treatment method and combined it with high-performance liquid chromatography-tandem mass spectrometry to test six herbicides (metamitron, clopyralid, desmedipham, phenmedipham, ethofumesate, and haloxyfop-p-methyl) in sugar beet plants, soil, and roots. The degradation dynamics and terminal residues of each herbicide in sugar beets were analysed. Finally, the dietary risks of various herbicides in sugar beets were evaluated based on the dietary structure of Chinese people, and the risk quotient values were below 100%. Using this detection method, all reagents exhibited good linearity (0.9724 ≤ R2 ≤ 0.9998), The limit of quantification (LOQ) ranged from 0.01 to 0.05 mg/L, the matrix effect ranged from -1.2% to -50%, the addition recovery rate ranged from 77.00% to 103.48%, and the relative standard deviation ranged from 1.61% to 16.17%; therefore, all indicators of this method met the residue detection standards. Under field conditions, the half-lives (t1/2) ranged about 0.65 ∼ 2.96 d and 0.38 ∼ 27.59 d in sugar beet plants and soil, respectively. All herbicides were easily degraded in sugar beet plants and soil (t1/2 < 30 d). The terminal residue amounts in the beet plants, soil, and roots ranged from < LOQ to 0.243 mg/kg. The dietary risk assessment of each pesticide was conducted based on the residual median of the terminal residues and the highest residual values on the edible part of the beetroot. The chronic exposure risk quotient (RQc) and acute exposure risk quotient (RQa) values were < 100%, indicating that the residue of each pesticide in beetroot posed low risks to consumers in China at the recommended dosage.


Assuntos
Beta vulgaris , Compostos de Flúor , Herbicidas , Resíduos de Praguicidas , Praguicidas , Piridinas , China , Herbicidas/análise , Resíduos de Praguicidas/análise , Praguicidas/análise , Solo/química , Açúcares , Verduras
3.
Sci Rep ; 13(1): 5814, 2023 Apr 10.
Artigo em Inglês | MEDLINE | ID: mdl-37037846

RESUMO

Propaquizafop is a fatty acid synthetic herbicide used to control annual and perennial grasses. To understand the potential environmental risks of propaquizafop to crops and food safety, the adsorption, mobility, and degradation of propaquizafop in five different soils were studied. At an initial concentration of 5 mg L-1 propaquizafop, its adsorption equilibrium was reached within 24 h, and the adsorption rates were between 46.98 and 57.76%. The Elovich kinetic model provided the best fit for the kinetic model, with R2 values between 0.9882 and 0.9940. For the isothermal adsorption tests, the Freundlich model was used to better fit the adsorption characteristics of propaquizafop in different soils, with R2 values between 0.9748 and 0.9885. Increasing the concentration of Ca2+ was beneficial for propaquizafop adsorption. In the soil thin-layer chromatography tests, the Rf of propaquizafop in the five soil samples ranged from 0.076 to 0.123. The results of the soil column leaching tests showed that propaquizafop did not migrate in the five soil columns; it was not detected in the leachate of each soil column, and propaquizafop in the soil columns only existed in the 0-5 cm soil layer. The results of soil thin-layer chromatography and soil column leaching tests showed that propaquizafop is a pesticide with a weak migration ability. Under the same environmental conditions, the degradation rate of propaquizafop in different soils followed the order LF fluvo-aquic soil (T1/2 = 1.41 d) > CS red loam (T1/2 = 2.76 d) > SX paddy soil (T1/2 = 3.52 d) > CC black soil (T1/2 = 5.74 d) > BS ginseng soil (T1/2 = 7.75 d). Considering the effects of soil moisture, incubation temperature, and microorganisms on propaquizafop degradation in the soil, temperature was found to have the greatest influence on its degradation rate.

4.
Environ Sci Pollut Res Int ; 30(10): 26367-26374, 2023 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-36357760

RESUMO

Mandipropamid, a new fungicide for oomycete disease, has a strong effect on the blight of many crops and has been registered for the treatment of ginseng blight in China. However, no maximum residue limit (MRL) of mandipropamid has been identified for ginseng, and there have been few related studies. We established and verified the analysis method of mandipropamid in ginseng using high-performance liquid chromatography-tandem mass spectrometry. The method has good linearity and accuracy in the range of 0.002-0.5 mg/kg. The average recovery of mandipropamid was 87.4-101.6%, and the standard deviation was 1.1-4.0. Mandipropamid in ginseng plants and soil rapidly degraded following first-order kinetics models. The degradation dynamics showed that the half-life of mandipropamid in ginseng plant and soil was 13.8-28.0 and 9.8-27.4 d, respectively. After the recommended dose of mandipropamid was applied once, the residual content of mandipropamid in fresh ginseng, dried ginseng, red ginseng, ginseng plant, and ginseng soil was < 0.01-0.185, < 0.01-0.265, 0.085-1.544, 0.075-4.800, and < 0.01-0.014 mg/kg, respectively. The dietary risk assessment of mandipropamid on ginseng showed that the risk quotient value was far less than 100%, indicating that the recommended dose of mandipropamid does not cause unacceptable risks to humans. After the recommended dose of mandipropamid was applied once, it did not cause unacceptable risks to humans. This study not only provides a reasonable spray dosage of mandipropamid to ginseng but also offers a reference for the establishment of MRLs in China.


Assuntos
Panax , Resíduos de Praguicidas , Humanos , China , Cromatografia Líquida de Alta Pressão/métodos , Panax/química , Resíduos de Praguicidas/análise , Medição de Risco , Espectrometria de Massas em Tandem/métodos , Exposição Dietética , Poluentes do Solo/análise
5.
Molecules ; 27(23)2022 Dec 02.
Artigo em Inglês | MEDLINE | ID: mdl-36500554

RESUMO

In this study, the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method, combined with high-performance liquid chromatography−tandem mass spectrometry, was chosen for detecting pydiflumetofen residues in soybean plants, soybeans and soil, and assessing the risk of short- and long-term dietary intake. Pydiflumetofen concentrations ranging from 0.001−0.5 mg/L exhibited good linearity (r > 0.997). At varying doses, the average pydiflumetofen recovery rates and relative standard deviations among soybean plants, soybeans, and soil ranged from 83.9 ± 1.1% to 99.5 ± 3.3% and from 0.77 to 7.77%, respectively. The sensitivity, accuracy, and precision of the chosen methodology met the requirements of pesticide residue analysis. The results of the degradation dynamics test showed that the half-life of pydiflumetofen (t1/2) in soybean plants and in soil were 3.6 to 5.7 and from 7.9 to 25.7 d, respectively. Assessment of the concentration of pydiflumetofen residues in soybeans revealed acute and chronic dietary exposure risks of 0.06 and 7.54%, respectively. As these values are very low, pydiflumetofen residues in soybeans present an acceptable risk to public health. The results of this study will help to guide the practical application of pydiflumetofen and minimize the environmental risks associated with its use.


Assuntos
Resíduos de Praguicidas , Espectrometria de Massas em Tandem , Espectrometria de Massas em Tandem/métodos , Resíduos de Praguicidas/análise , Solo/química , Medição de Risco , Meia-Vida
6.
Environ Sci Process Impacts ; 24(12): 2465-2474, 2022 Dec 14.
Artigo em Inglês | MEDLINE | ID: mdl-36445190

RESUMO

The study of the adsorption properties of pesticides in soil is essential to assessing the risk of their pollution of nearby aquatic environments. To reveal the adsorption mechanisms of flupyradifurone (FPO) on soil, batch experiments in five different soils were carried out in this study. The adsorption kinetics and isotherms of FPO in five soils were well fitted by using several models (R2 = 0.922-0.998). It was found that both physical and chemical adsorption were included in the adsorption process of FPO in soils; the monolayer adsorption of FPO occurred with a non-uniform energy distribution on the soil surface, and the internal particle diffusion was not the only rate-controlling step. The adsorption coefficients calculated by using the Langmuir (KL) and Freundlich (KF) models were 0.0158-0.0982 and 1.053-9.798, respectively. In addition, the main factors affecting the adsorption of FPO in soil were investigated by stepwise regression fitted with the adsorption coefficient (Kd) and the soil properties. It was found that the organic carbon content was the main factor (R2 = 0.857, p < 0.05). Therefore, the organic carbon adsorption coefficients (Koc) were calculated. The results (1.0532-5.6529) indicated that FPO has a low affinity and high mobility in the soils, and may cause water environment pollution around the soil. Therefore, FPO should be used cautiously in paddy fields. These research findings were important for elucidating the sorption behaviour and transport of FPO in soil.


Assuntos
Poluentes do Solo , Solo , Solo/química , Adsorção , Poluentes do Solo/análise , Cinética , Carbono/química
7.
Molecules ; 27(17)2022 Aug 26.
Artigo em Inglês | MEDLINE | ID: mdl-36080241

RESUMO

The massive use of pesticides has brought great risks to food and environmental safety. It is necessary to develop reliable analytical methods and evaluate risks through monitoring studies. Here, a method was used for the simultaneous determination of flupyradifurone (FPF) and its two metabolites in fresh ginseng, dried ginseng, ginseng plants, and soil. The method exhibited good accuracy (recoveries of 72.8-97.5%) and precision (relative standard deviations of 1.1-8.5%). The field experiments demonstrated that FPF had half-lives of 4.5-7.9 d and 10.0-16.9 d in ginseng plants and soil, respectively. The concentrations of total terminal residues in soil, ginseng plants, dried ginseng, and ginseng were less than 0.516, 2.623, 2.363, and 0.641 mg/kg, respectively. Based on these results, the soil environmental risk assessment shows that the environmental risk of FPF to soil organisms is acceptable. The processing factors for FPF residues in ginseng were 3.82-4.59, indicating that the concentration of residues increased in ginseng after drying. A dietary risk assessment showed that the risk of FPF residues from long-term and short-term dietary exposures to global consumers were 0.1-0.4% and 12.07-13.16%, respectively, indicating that the application of FPF to ginseng at the recommended dose does not pose a significant risk to consumers.


Assuntos
Panax , Resíduos de Praguicidas , Poluentes do Solo , 4-Butirolactona/análogos & derivados , Monitoramento Ambiental/métodos , Panax/química , Resíduos de Praguicidas/análise , Piridinas , Medição de Risco , Solo/química , Poluentes do Solo/análise
8.
Sci Total Environ ; 836: 155448, 2022 Aug 25.
Artigo em Inglês | MEDLINE | ID: mdl-35508239

RESUMO

In the present study, aqueous behavior and fate of diamide insecticide tetrachlorantraniliprole (TCTP) were investigated under laboratory-controlled conditions. Half-lives of TCTP photolysis in natural water and pH buffers were 1.4-2.8 h, comparing with those of 1.2-231 d for hydrolysis. Both processes were highly influenced by pH with respect to degradation kinetics and routes. The hydrolysis rate of TCTP was accelerated by elevated temperatures. The presence of nitrate enhanced TCTP photolysis while fulvic acid exhibited suppression, with the extent of both effects as a function of concentration. Four degradation products were identified using a variety of spectroscopic approaches. Key reactions involved in the degradation pathways include intramolecular substitution and cyclization. There was a reduction in the acute toxicity of all four products to Daphnia magna by comparison with TCTP, whereas they were still classified as category 1 or 2 hazardous substances to the aquatic environment according to the Globally Harmonized System of Classification and Labelling of Chemicals (GHS) standards.


Assuntos
Inseticidas , Poluentes Químicos da Água , Diamida , Inseticidas/toxicidade , Cinética , Fotólise , Água/química , Poluentes Químicos da Água/análise
9.
Chemosphere ; 298: 134294, 2022 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-35283145

RESUMO

Flupyradifurone (FPO) easily spreads to the water environment after application because of its high solubility in water (3200 mg/L, 20 °C), but as a novel neonicotinoid pesticide, its environmental fate study is still lacking. Here, laboratory experiments were conducted to investigate the degradation kinetics and pathways of FPO in aqueous solutions and natural waters. The results showed that FPO was fairly stable in water under natural conditions (the hydrolysis half-lives at 15 °C, 25 °C, and 35 °C were >150 d, and the photolysis half-lives under sunlight were >168 h). However, FPO was photodegraded rapidly under ultraviolet (UV) light (half-lives of 2.37-3.81 min). Then, indirect photolysis under UV light was examined with the addition of photosensitizers, revealing that direct photolysis is the main FPO degradation pathway in water, and the contribution of indirect photolysis was limited. Moreover, two photoproducts were separated, purified and collected via preparative HPLC, and identified via high resolution mass spectrometry. Then, the plausible photolysis pathway was proposed. The results of this study will contribute to a better understanding of the fate of FPO in the water environment.


Assuntos
Poluentes Químicos da Água , Água , 4-Butirolactona/análogos & derivados , Hidrólise , Cinética , Fotólise , Piridinas , Água/química , Poluentes Químicos da Água/análise
10.
J Anal Methods Chem ; 2022: 4208243, 2022.
Artigo em Inglês | MEDLINE | ID: mdl-35223127

RESUMO

Ginseng is a perennial herb with a long growth cycle and is known to easily accumulate pesticides during its growth process, seriously threatening people's health. Therefore, to ensure safe consumption, it is necessary to detect and monitor pesticide residues in ginseng. In this study, a novel analysis method was established for simultaneous determination of 31 pesticides in ginseng by high-performance liquid chromatography-mass spectrometry. Ginseng samples were extracted using acetonitrile, cleaned up by primary secondary amine (PSA) solid-phase extraction column eluted with acetonitrile-toluene, and then detected in multiple reaction mode (MRM). The calibration curves of target compounds were linear in the range of 0.005-1.0 mg/L, with correlation coefficients greater than 0.9921. The limits of detection of all the pesticides in ginseng were between 4.4×10-5 and 1.6 × 10-2 mg/kg. For fresh ginseng, the average recoveries ranged from 72.1 to 111.6%, and the relative standard deviations were 1.3-12.2%. For dry ginseng, the average recoveries were 74.3-108.3%, and the relative standard deviations were 0.9-14.9%. The residual concentrations of some pesticides in real samples were greater than the maximum residue limit (MRL) for European Union (EU). The method established here is rapid and simple with high sensitivity and good reproducibility, which is sensitive in the residue analysis of many pesticides in ginseng.

11.
J Environ Sci Health B ; 56(12): 1042-1050, 2021.
Artigo em Inglês | MEDLINE | ID: mdl-34846269

RESUMO

In the present study, an analytical method that combined a modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method and high-performance liquid chromatography coupled with tandem mass spectrometry was developed to determine trifluorocide in fresh and dried ginseng roots, plants (stems and leaves), and soil. At three spiked levels (0.01, 0.1, and 1.0 mg kg-1), the mean recoveries (n = 15) of trifluorocide from fresh and dried ginseng roots, plants, and soil were in the range of 95.6 - 109.7%, with relative standard deviations less than 10.0%. The limits of quantitation of different matrices were determined to be 0.01 mg kg-1. Dissipation and residue study of trifluorocide was conducted in ginseng cultivation ecosystems in Northeast China. The t1/2 (half-life) of trifluorocide in ginseng fresh roots, plants, and soil were 8.3-13.1 days, 7.4-10.9 days, and 8.8-10.6 days, respectively. The terminal residues of trifluorocide in ginseng fresh roots were less than 0.01 mg kg-1 after 35 days of trifluorocide application. This study could be beneficial in residue analysis and assist in the scientific application of trifluorocide during ginseng cultivation.


Assuntos
Panax , Resíduos de Praguicidas , Poluentes do Solo , Cromatografia Líquida de Alta Pressão , Ecossistema , Monitoramento Ambiental/métodos , Meia-Vida , Panax/química , Resíduos de Praguicidas/análise , Solo/química , Poluentes do Solo/análise , Espectrometria de Massas em Tandem/métodos
12.
J Anal Methods Chem ; 2021: 5516563, 2021.
Artigo em Inglês | MEDLINE | ID: mdl-34422433

RESUMO

In this study, an analytical method was developed for the rapid determination of 21 pesticides used in ginseng cultivation. All pesticides covered by this method have been registered by 2020 in China for use on ginseng. The extracts were cleaned up using zirconium-oxide-modified silica (Z-Sep) and primary secondary amine (PSA). The combination of Z-Sep and PSA provided good recovery for all analytes and the cleanest matrix background out of a number of PSA-based sorbent combinations, as indicated by high-performance liquid chromatography (HPLC) and gas chromatography (GC). Instrumental analysis was completed in 5 min using the ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The linearity (r > 0.99) for all analytes was satisfactory over the calibration range of 0.002-0.1 µg mL-1. Intraday recoveries (n = 5) at ginseng-spiked levels of 0.02, 0.05, 0.1, and 1 mg kg-1 ranged between 72% and 119%, with the corresponding relative standard deviations (RSDs), were less than 19%, while the interday recoveries (n = 15) ranged between 77% and 103%, and RSDs were less than 22%. Limits of quantitation (LOQs) ranged between 0.02 and 0.05 mg kg-1 for all 21 pesticides. This is a seminal study using Z-Sep for the efficient cleanup of ginseng samples, and it could present a practical method for future monitoring of pesticide residues in ginseng produced in China.

13.
Bull Environ Contam Toxicol ; 105(4): 602-606, 2020 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-32978647

RESUMO

A method for simultaneous quantitation of rimsulfuron, quizalofop-P-ethyl and quizalofop-P in potato plant, soil and potato tuber samples was established. The mean recoveries of rimsulfuron, quizalofop-P-ethyl and quizalofop-P in different matrices spiked with them were 81.4%-101.1%, 76.1%-99.0% and 77.4%-106.4% with relative standard deviations (RSDs) of 2.7%-13.3%, 0.9%-5.5%, 1.7%-11.3%, respectively. The open-field trials in China were conducted in potato cultivation system of Changchun and Jinan. The results indicated that the half-lives of rimsulfuron and quizalofop-P-ethyl were 0.04-13.1 days. The residues of quizalofop-P during the harvest time in Jinan soil were < 0.01-0.044 mg kg-1, while there was no residue of target herbicides detected in all other samples. The risk assessment results demonstrated that the risk quotients (RQs) of rimsulfuron and quizalofop-P-ethyl were 7.857 × 10-5 and 8.730 × 10-3, respectively, which exhibited an acceptable dietary risk to Chinese consumers.


Assuntos
Resíduos de Praguicidas/análise , Propionatos/análise , Piridinas/análise , Quinoxalinas/análise , Poluentes do Solo/análise , Sulfonamidas/análise , China , Herbicidas/análise , Medição de Risco , Solo/química , Solanum tuberosum
14.
J Chromatogr A ; 1620: 461004, 2020 Jun 07.
Artigo em Inglês | MEDLINE | ID: mdl-32143875

RESUMO

In the present study, a fast multiresidue method determining three novel fungicides fenpicoxamid, isofetamid, and mandestrobin in cereals was developed and validated for the first time using ultrahigh-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Samples were extracted by QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) methodology, and cleaned up using the disposable pipette extraction (DPX) tips containing primary secondary amine (PSA) and silica gel modified with zirconium oxide (Z-Sep) in less than 1 min. Linearity (r > 0.99) of three fungicides in the calibration range of 0.001-0.1 µg mL-1 was satisfactory. Mean recoveries (n = 15) from all matrices were between 84.8% and 100.3% as the corresponding intra-day and inter-day relative standard deviations (RSDs) were less than 10.6%. Limits of quantitation (LOQs) of all analytes in different matrices were defined at 0.01 mg kg-1. The results indicate this method can serve as a sensitive and rapid approach to monitoring contents of fenpicoxamid, isofetamid, and mandestrobin in cereals.


Assuntos
Acetamidas/análise , Cromatografia Líquida de Alta Pressão/métodos , Grão Comestível/química , Fungicidas Industriais/análise , Resíduos de Praguicidas/análise , Espectrometria de Massas em Tandem/métodos , Tiofenos/análise , Fracionamento Químico/instrumentação , Fungicidas Industriais/química , Fungicidas Industriais/isolamento & purificação , Lactonas/análise , Lactonas/química , Lactonas/isolamento & purificação , Resíduos de Praguicidas/química , Resíduos de Praguicidas/isolamento & purificação , Piridinas/análise , Piridinas/química , Piridinas/isolamento & purificação , Zircônio/química
15.
J Environ Sci Health B ; 55(6): 566-573, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-32174229

RESUMO

Tomatoes have been widely planted in greenhouses and fields in China. Soil-borne diseases are more harmful to tomatoes than other types of diseases. Dimethyl disulfide (DMDS) was used as a novel fumigant instead of methyl bromide to control soil-borne diseases. To assess the safety of DMDS for use on tomatoes, its dissipation and terminal residues were investigated at three different locations under greenhouse and open field conditions. The QuEChERS method was simplified using gas chromatography with mass spectrometry detection and combined with liquid-liquid extraction purification to allow determination of DMDS levels in both the tomatoes and the soil. The average recovery of the method was between 85.3 and 98.6%, with the relative standard deviation (RSD) ranging from to 1.9-10.3%. The dissipation and terminal residues of DMDS in the tomatoes and the soil were analyzed using the method, the results of which showed that the half-life of DMDS ranged from 0.3-6.5 d in the soil at three different locations. The terminal residues of DMDS in the tomatoes and the soil were not detected. This study provided data that the Chinese government can use to support appropriate and safe guidance for the use of DMDS on agriculture.


Assuntos
Dissulfetos/química , Resíduos de Praguicidas/análise , Poluentes do Solo/análise , Solanum lycopersicum/química , Agricultura/métodos , China , Dissulfetos/análise , Cromatografia Gasosa-Espectrometria de Massas , Meia-Vida , Extração Líquido-Líquido , Solo/química , Poluentes do Solo/química
16.
Int J Anal Chem ; 2020: 8812797, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-33628252

RESUMO

In this study, an analytical method for the simultaneous determination of the novel insecticide flupyradifurone and its two metabolites in a variety of traditional Chinese herbal medicines was developed for the first time using high-performance liquid chromatography-tandem mass spectrometry. A simple and efficient method using dispersive solid-phase extraction was employed for the pretreatment of the samples. Several extractions and cleanup strategies were evaluated. The recoveries (n = 15) of flupyradifurone and its metabolites at three spiking levels were in the range 71.3%-101.7%, with corresponding intraday and interday relative standard deviations of 1.1%-14.8%. The limits of quantitation were 0.01 mg/kg for flupyradifurone and 0.1 mg/kg for its two metabolites. Overall, our developed method was sensitive and reliable for the fast screening of flupyradifurone and its two metabolites in traditional Chinese herbal medicine samples.

17.
J Agric Food Chem ; 67(39): 10977-10983, 2019 Oct 02.
Artigo em Inglês | MEDLINE | ID: mdl-31490679

RESUMO

In this study, an analytical method was developed and validated for simultaneous determination of five diamide insecticides (chlorantraniliprole, cyantraniliprole, flubendiamide, cyclaniliprole, and tetrachlorantraniliprole) in food matrices. Determination of the latter two diamide compounds is first reported. Samples were cleaned up by multiplug filters containing carbon nanotubes (CNT) or hydrophilic-lipophilic balanced copolymers (HLB) and classic dispersive solid phase extraction (d-SPE) procedures, respectively. The CNT multiplug filter performed the best in terms of process rapidity and cleanup efficiency; thus, it was finally chosen for sample cleanup. Instrumental analysis was completed in 5 min using ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Mean recoveries of the five diamides ranged from 84.3 to 110.0%, with intraday and interday relative standard deviations (RSD) of less than 13.5%. Limits of quantitation (LOQ) of all analytes ranged from 0.005 to 0.01 mg kg-1 in different matrices. The results indicate this method is reliable for monitoring the five diamide insecticides in various foods.


Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Diamida/química , Filtração/métodos , Contaminação de Alimentos/análise , Inseticidas/química , Resíduos de Praguicidas/química , Espectrometria de Massas em Tandem/métodos , Diamida/isolamento & purificação , Filtração/instrumentação , Inseticidas/isolamento & purificação , Nanotubos de Carbono/química , Resíduos de Praguicidas/isolamento & purificação
18.
Artigo em Inglês | MEDLINE | ID: mdl-31561447

RESUMO

The widespread use of fluazifop-p-butyl (FPB) contributes to its presence in the environment. Considering the ecological risks of FPB residues in the environment, the anatase nanometer titanium dioxide (nano-TiO2) mediated photocatalytic degradation of FPB was studied by smearing FPB and nano-TiO2 together on a glass plane; illumination, trimethylsilane derivatization of photolysis products, high performance liquid chromatography (HPLC) quantitative analysis and gas chromatograph-mass spectrometer (GC-MS) identification were used. Results showed that the first order dynamic model could describe the photodegradation of FPB by nano-TiO2 mediated, and the photodegradation and photosensitization rates were found to be positively correlated with the dose of nano-TiO2 at lower dose ranges. It is noticeable that a strong photosensitization effect was exhibited on degradation of FPB, not only under high-pressure mercury lamps, but also simulated sunlight (xenon lamp light). Ultimately, twelve main photolytic products were reasonably speculated, whilst five photolysis pathways were proposed. These results together suggest that nano-TiO2 can be used as an effective photosensitizer to accelerate FPB photolysis.


Assuntos
Catálise , Recuperação e Remediação Ambiental/métodos , Herbicidas/química , Fotólise , Piridinas/química , Luz Solar , Titânio/química
19.
Environ Monit Assess ; 189(11): 534, 2017 Oct 02.
Artigo em Inglês | MEDLINE | ID: mdl-28971277

RESUMO

Ginseng is a valuable herb, the roots of which have been consumed for medicinal use since ancient times in Asian countries. Currently, its cultivation in China is conducted in either forests or non-forest areas. In this study, we investigated the dissipation and residues of the diamide insecticide chlorantraniliprole (CAP) in ginseng ecosystems in these two cultivation environments. The half-life of CAP in ginseng leaves was calculated to be 16.5 days in non-forest areas and 23.9 days in forests, while the half-life of CAP in the soil under non-forest and forest cultivation was 33.0 and 53.3 days, respectively. The relatively long persistence of CAP in ginseng leaves and soil could be attributed to the unique cultivation techniques of ginseng, which prevents exposure to direct sunlight irradiation and rainfall. The residual amounts of CAP in ginseng leaves, roots, and soil in non-forest areas were 0.168, 0.011, and 0.013 mg kg-1 21 days after CAP application at the maximum label-allowed dosage and frequency versus 0.564, 0.013, and < 0.005 mg kg-1 in forests. CAP application strategies for the control of Lepidoptera pests such as armyworms, and the safety of harvested ginseng roots are recommended for ginseng cultivated in forests and non-forest areas based on the results of the CAP residue experiments.


Assuntos
Monitoramento Ambiental , Inseticidas/análise , Panax/química , Resíduos de Praguicidas/análise , ortoaminobenzoatos/análise , Ásia , China , Diamida , Ecossistema , Florestas , Meia-Vida , Folhas de Planta/química , Raízes de Plantas/química , Solo/química , Poluentes do Solo/análise
20.
Pestic Biochem Physiol ; 134: 63-72, 2016 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-27914541

RESUMO

Panax ginseng C.A. Meyer is a valuable herb in China that has also gained popularity in the West because of its pharmacological properties. The constituents isolated and characterized in ginseng stems include ginsenosides, fatty acids, amino acids, volatile oils, and polysaccharides. In this study, the effects of fungicide azoxystrobin applied on antioxidant enzyme activity and ginsenosides content in ginseng stems was studied by using Panax ginseng C. A. Mey. cv. (the cultivar of Ermaya) under natural environmental conditions. The azoxystrobin formulation (25% SC) was sprayed three times on ginseng plants at different doses (150ga.i./ha and 225ga.i./ha), respectively. Two new fatty acids esters (ethyl linoleate and methyl linolenate) were firstly detected in ginseng stems by the application of azoxystrobin as foliar spray. The results indicated that activities of enzymatic antioxidants, the content of ginsenosides and two new fatty acids esters in ginseng stems in azoxystrobin-treated plants were increased. Azoxystrobin treatments to ginseng plants at all growth stages suggest that the azoxystrobin-induced delay of senescence is due to an enhanced antioxidant enzyme activity protecting the plants from harmful active oxygen species (AOS). The activity of superoxide dismutase (SOD) in azoxystrobin-treated plants was about 1-3 times higher than that in untreated plants. And the effects was more significant (P=0.05) when azoxystrobin was applied at dose of 225ga.i./ha. This work suggests that azoxystrobin plays an important role in delaying of senescence by changing physiological and biochemical indicators and increasing ginsenosides content in ginseng stems.


Assuntos
Fungicidas Industriais/farmacologia , Ácidos Linoleicos/metabolismo , Ácidos Linolênicos/metabolismo , Metacrilatos/farmacologia , Panax/efeitos dos fármacos , Caules de Planta/efeitos dos fármacos , Pirimidinas/farmacologia , Ascorbato Peroxidases/metabolismo , Catalase/metabolismo , Clorofila/metabolismo , Ésteres , Ginsenosídeos/metabolismo , Peróxido de Hidrogênio/metabolismo , Malondialdeído/metabolismo , Panax/química , Panax/metabolismo , Peroxidase/metabolismo , Proteínas de Plantas/metabolismo , Caules de Planta/química , Caules de Planta/metabolismo , Estrobilurinas , Superóxido Dismutase/metabolismo , Superóxidos/metabolismo
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