吡咯苯脲在水稻和稻田环境中的降解动态和残留测定。

Q3 Medicine
H Wu, J Wang, K Yang, X Wang, N Fang, L Duan, C Zhang, X Wang
{"title":"吡咯苯脲在水稻和稻田环境中的降解动态和残留测定。","authors":"H Wu, J Wang, K Yang, X Wang, N Fang, L Duan, C Zhang, X Wang","doi":"10.16250/j.32.1915.2024164","DOIUrl":null,"url":null,"abstract":"<p><strong>Objective: </strong>To establish a method for determination of pyriclobenzuron (PBU) residues in rice and paddy environments, and to determine the residual amounts and observe the degradation dynamics of PBU.</p><p><strong>Methods: </strong>In July 2022, the paddies of Zhejiang Academy of Agricultural Sciences were selected as experimental fields, and were divided into the blank control group (no pesticide application), the 1-fold-concentration pesticide group (1 kg/667 m<sup>2</sup>), and the 5-fold-concentration pesticide group (5 kg/667 m<sup>2</sup>), with a 100 m<sup>2</sup> area in each group. At the early tillering stage of rice, 20% suspension of PBU sulfate was sprayed once in the 1-fold-concentration and 5-fold-concentration pesticide groups, and rice plants, paddy water and soil samples were collected 2 h, and 1, 2, 3, 5, 7, 11, 14, 21, 28, 35, 49 d and 63 d following spraying PBU, while rice straw, field soil, brown rice and rice husk samples were collected 98 d following spraying. PBU was extracted and purified in samples using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) pretreatment technique, and the PBU contents were determined in samples using ultrahigh performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The solvent standard working solution and matrix standard working solution were prepared. A linear regression equation was fitted between PBU concentration (x-axis) and peak area (y-axis), and the ratio of the slope (<i>k</i>) of the matrix standard curve to the slope (<i>K</i>) of the solvent standard curve was calculated to evaluate the matrix effect of PBU in samples. According to the <i>Guidelines for Pesticide Residue Testing in Crops (NY/T 788</i>-<i>2018)</i>, the addition levels of PBU were set at 0.005, 0.050, 5.000, 1 000.000 mg/kg in rice plants, 0.005, 0.050, 2.000, 10.000 mg/kg in paddy water, 0.005, 0.050, 2.000 mg/kg in soil, and 0.005, 0.050, 5.000 mg/kg in brown rice and rice husks. The recovery and relative standard deviation (RSD) of PBU addition were calculated to evaluate the effectiveness of UPLC-MS/MS for determination of PBU contents. The first-order kinetic equation of PBU concentration was fitted in samples at different sampling time points to analyze the trends in PBU degradation in rice plants, paddy water, and soil, and the half-life of PBU was calculated in different samples.</p><p><strong>Results: </strong>There was a good linear relationship between the mass concentration and peak area of PBU at concentrations of 0.000 1 to 0.020 0 mg/kg under solvent and matrix conditions (<i>R</i><sup>2</sup> = 0.985 8 to 0.999 7, <i>t</i> = -0.47 to 1.62, all <i>P</i> values < 0.01). The matrix effects of PBU were 70.26%, 65.42% and 65.12% in rice plants, brown rice and rice husks, indicating a matrix-inhibitory effect, and the matrix effect was 87.06% in soils, indicating a weak matrix effect. The recovery of PBU addition was 77.61% to 100.12% in different samples, with RSD of 1.43% to 6.74%, and a limit of quantification (LOQ) of 0.005 mg/kg, and the addition recovery and RSD met the requirements of the Guidelines for Pesticide Residue Testing in Crops (NY/T 788-2018), validating the effectiveness of UPLC-MS/MS assay. Following spraying PBU at a dose of 1 kg/667 m<sup>2</sup>, the half-life of PBU was 6.24 d in rice plants and 3.43 d in paddy water samples, respectively. The final residues of PBU were lower than the LOQ of 0.005 mg/kg in brown rice and rice husk samples 98 d following spraying PBU. Following spraying PBU at a dose of 5 kg/667 m<sup>2</sup>, the half-life of PBU was 15.75 d in rice plants and 7.62 d in paddy water samples, respectively. The final residue of PBU was lower than the LOQ of 0.005 mg/kg in brown rice 98 d following spraying PBU, and the final residue of PBU was 0.049 mg/kg in rice husks.</p><p><strong>Conclusions: </strong>A simple, and highly accurate and precise UPLC-MS/MS assay has been developed for determination of PBU residues in rice plants and paddy environments through extraction and purification of PBU from matrix samples using QuEChERS pretreatment. After spraying PBU in paddies, the concentration of PBU gradually decreases in rice plants and paddy water over time, and the final residual concentration is low.</p>","PeriodicalId":38874,"journal":{"name":"中国血吸虫病防治杂志","volume":"37 2","pages":"201-208"},"PeriodicalIF":0.0000,"publicationDate":"2025-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"[Degradation dynamics and residue determination of pyriclobenzuron in rice and paddy environments].\",\"authors\":\"H Wu, J Wang, K Yang, X Wang, N Fang, L Duan, C Zhang, X Wang\",\"doi\":\"10.16250/j.32.1915.2024164\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><strong>Objective: </strong>To establish a method for determination of pyriclobenzuron (PBU) residues in rice and paddy environments, and to determine the residual amounts and observe the degradation dynamics of PBU.</p><p><strong>Methods: </strong>In July 2022, the paddies of Zhejiang Academy of Agricultural Sciences were selected as experimental fields, and were divided into the blank control group (no pesticide application), the 1-fold-concentration pesticide group (1 kg/667 m<sup>2</sup>), and the 5-fold-concentration pesticide group (5 kg/667 m<sup>2</sup>), with a 100 m<sup>2</sup> area in each group. At the early tillering stage of rice, 20% suspension of PBU sulfate was sprayed once in the 1-fold-concentration and 5-fold-concentration pesticide groups, and rice plants, paddy water and soil samples were collected 2 h, and 1, 2, 3, 5, 7, 11, 14, 21, 28, 35, 49 d and 63 d following spraying PBU, while rice straw, field soil, brown rice and rice husk samples were collected 98 d following spraying. PBU was extracted and purified in samples using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) pretreatment technique, and the PBU contents were determined in samples using ultrahigh performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The solvent standard working solution and matrix standard working solution were prepared. A linear regression equation was fitted between PBU concentration (x-axis) and peak area (y-axis), and the ratio of the slope (<i>k</i>) of the matrix standard curve to the slope (<i>K</i>) of the solvent standard curve was calculated to evaluate the matrix effect of PBU in samples. According to the <i>Guidelines for Pesticide Residue Testing in Crops (NY/T 788</i>-<i>2018)</i>, the addition levels of PBU were set at 0.005, 0.050, 5.000, 1 000.000 mg/kg in rice plants, 0.005, 0.050, 2.000, 10.000 mg/kg in paddy water, 0.005, 0.050, 2.000 mg/kg in soil, and 0.005, 0.050, 5.000 mg/kg in brown rice and rice husks. The recovery and relative standard deviation (RSD) of PBU addition were calculated to evaluate the effectiveness of UPLC-MS/MS for determination of PBU contents. The first-order kinetic equation of PBU concentration was fitted in samples at different sampling time points to analyze the trends in PBU degradation in rice plants, paddy water, and soil, and the half-life of PBU was calculated in different samples.</p><p><strong>Results: </strong>There was a good linear relationship between the mass concentration and peak area of PBU at concentrations of 0.000 1 to 0.020 0 mg/kg under solvent and matrix conditions (<i>R</i><sup>2</sup> = 0.985 8 to 0.999 7, <i>t</i> = -0.47 to 1.62, all <i>P</i> values < 0.01). The matrix effects of PBU were 70.26%, 65.42% and 65.12% in rice plants, brown rice and rice husks, indicating a matrix-inhibitory effect, and the matrix effect was 87.06% in soils, indicating a weak matrix effect. The recovery of PBU addition was 77.61% to 100.12% in different samples, with RSD of 1.43% to 6.74%, and a limit of quantification (LOQ) of 0.005 mg/kg, and the addition recovery and RSD met the requirements of the Guidelines for Pesticide Residue Testing in Crops (NY/T 788-2018), validating the effectiveness of UPLC-MS/MS assay. Following spraying PBU at a dose of 1 kg/667 m<sup>2</sup>, the half-life of PBU was 6.24 d in rice plants and 3.43 d in paddy water samples, respectively. The final residues of PBU were lower than the LOQ of 0.005 mg/kg in brown rice and rice husk samples 98 d following spraying PBU. Following spraying PBU at a dose of 5 kg/667 m<sup>2</sup>, the half-life of PBU was 15.75 d in rice plants and 7.62 d in paddy water samples, respectively. The final residue of PBU was lower than the LOQ of 0.005 mg/kg in brown rice 98 d following spraying PBU, and the final residue of PBU was 0.049 mg/kg in rice husks.</p><p><strong>Conclusions: </strong>A simple, and highly accurate and precise UPLC-MS/MS assay has been developed for determination of PBU residues in rice plants and paddy environments through extraction and purification of PBU from matrix samples using QuEChERS pretreatment. After spraying PBU in paddies, the concentration of PBU gradually decreases in rice plants and paddy water over time, and the final residual concentration is low.</p>\",\"PeriodicalId\":38874,\"journal\":{\"name\":\"中国血吸虫病防治杂志\",\"volume\":\"37 2\",\"pages\":\"201-208\"},\"PeriodicalIF\":0.0000,\"publicationDate\":\"2025-03-11\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"中国血吸虫病防治杂志\",\"FirstCategoryId\":\"3\",\"ListUrlMain\":\"https://doi.org/10.16250/j.32.1915.2024164\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"Medicine\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"中国血吸虫病防治杂志","FirstCategoryId":"3","ListUrlMain":"https://doi.org/10.16250/j.32.1915.2024164","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"Medicine","Score":null,"Total":0}
引用次数: 0

摘要

目的:建立稻谷环境中吡咯苯脲残留量的测定方法,测定其残留量并观察其降解动态。方法:于2022年7月选取浙江省农业科学院稻田作为试验田,分为空白对照组(不施用农药)、1倍浓度农药组(1 kg/667 m2)和5倍浓度农药组(5 kg/667 m2),每组面积100 m2。在水稻分蘖初期,在1倍浓度和5倍浓度农药组各喷一次20%硫酸pbu悬浮液,在喷施PBU后2 h和1、2、3、5、7、11、14、21、28、35、49和63 d采集水稻植株、水稻水和土壤样品,在喷施后98 d采集水稻秸秆、田间土壤、糙米和稻壳样品。采用快速、简便、廉价、有效、坚固、安全(QuEChERS)预处理技术提取和纯化样品中的PBU,并采用超高效液相色谱-串联质谱(UPLC-MS/MS)测定样品中的PBU含量。制备了溶剂标准工作液和基质标准工作液。拟合PBU浓度(x轴)与峰面积(y轴)之间的线性回归方程,计算基质标准曲线斜率(k)与溶剂标准曲线斜率(k)之比,评价样品中PBU的基质效应。根据《作物农药残留检测指南》(NY/T 788-2018),水稻中PBU的添加量分别为0.005、0.050、5.000、1000.000 mg/kg,水稻水中PBU的添加量分别为0.005、0.050、2.000、10.000 mg/kg,土壤中PBU的添加量分别为0.005、0.050、2.000 mg/kg,糙米和稻壳中PBU的添加量分别为0.005、0.050、5.000 mg/kg。计算添加PBU的回收率和相对标准偏差(RSD),评价UPLC-MS/MS法测定PBU含量的有效性。拟合了不同采样时间点样品中PBU浓度的一级动力学方程,分析了PBU在水稻植株、稻田水和土壤中的降解趋势,并计算了不同样品中PBU的半衰期。结果:在溶剂和基质条件下,PBU浓度为0.000 ~ 0.020 mg/kg时,质量浓度与峰面积呈良好的线性关系(R2 = 0.985 ~ 0.999 7, t = -0.47 ~ 1.62, P值均< 0.01)。PBU在水稻植株、糙米和稻壳中的基质效应分别为70.26%、65.42%和65.12%,具有基质抑制作用;在土壤中的基质效应为87.06%,基质效应较弱。PBU在不同样品中的添加回收率为77.61% ~ 100.12%,RSD为1.43% ~ 6.74%,定量限(LOQ)为0.005 mg/kg,添加回收率和RSD符合《作物农药残留检测指南》(NY/T 788-2018)的要求,验证了UPLC-MS/MS法的有效性。喷施PBU剂量为1 kg/667 m2后,PBU在水稻植株中的半衰期为6.24 d,在水稻水样中的半衰期为3.43 d。施用PBU 98 d后,糙米和稻壳样品中PBU的最终残留量均低于0.005 mg/kg的定量限。喷施5 kg/667 m2后,PBU在水稻植株中的半衰期为15.75 d,在水稻水样中的半衰期为7.62 d。施用PBU后98 d糙米中PBU的最终残留量低于限定限0.005 mg/kg,稻壳中PBU的最终残留量为0.049 mg/kg。结论:采用QuEChERS预处理技术从基质样品中提取纯化PBU,建立了一种简便、高精度的UPLC-MS/MS检测水稻植株和水稻环境中PBU残留量的方法。稻田喷洒PBU后,水稻植株和稻田水中PBU浓度随时间逐渐降低,最终残留浓度较低。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
[Degradation dynamics and residue determination of pyriclobenzuron in rice and paddy environments].

Objective: To establish a method for determination of pyriclobenzuron (PBU) residues in rice and paddy environments, and to determine the residual amounts and observe the degradation dynamics of PBU.

Methods: In July 2022, the paddies of Zhejiang Academy of Agricultural Sciences were selected as experimental fields, and were divided into the blank control group (no pesticide application), the 1-fold-concentration pesticide group (1 kg/667 m2), and the 5-fold-concentration pesticide group (5 kg/667 m2), with a 100 m2 area in each group. At the early tillering stage of rice, 20% suspension of PBU sulfate was sprayed once in the 1-fold-concentration and 5-fold-concentration pesticide groups, and rice plants, paddy water and soil samples were collected 2 h, and 1, 2, 3, 5, 7, 11, 14, 21, 28, 35, 49 d and 63 d following spraying PBU, while rice straw, field soil, brown rice and rice husk samples were collected 98 d following spraying. PBU was extracted and purified in samples using a quick, easy, cheap, effective, rugged, and safe (QuEChERS) pretreatment technique, and the PBU contents were determined in samples using ultrahigh performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The solvent standard working solution and matrix standard working solution were prepared. A linear regression equation was fitted between PBU concentration (x-axis) and peak area (y-axis), and the ratio of the slope (k) of the matrix standard curve to the slope (K) of the solvent standard curve was calculated to evaluate the matrix effect of PBU in samples. According to the Guidelines for Pesticide Residue Testing in Crops (NY/T 788-2018), the addition levels of PBU were set at 0.005, 0.050, 5.000, 1 000.000 mg/kg in rice plants, 0.005, 0.050, 2.000, 10.000 mg/kg in paddy water, 0.005, 0.050, 2.000 mg/kg in soil, and 0.005, 0.050, 5.000 mg/kg in brown rice and rice husks. The recovery and relative standard deviation (RSD) of PBU addition were calculated to evaluate the effectiveness of UPLC-MS/MS for determination of PBU contents. The first-order kinetic equation of PBU concentration was fitted in samples at different sampling time points to analyze the trends in PBU degradation in rice plants, paddy water, and soil, and the half-life of PBU was calculated in different samples.

Results: There was a good linear relationship between the mass concentration and peak area of PBU at concentrations of 0.000 1 to 0.020 0 mg/kg under solvent and matrix conditions (R2 = 0.985 8 to 0.999 7, t = -0.47 to 1.62, all P values < 0.01). The matrix effects of PBU were 70.26%, 65.42% and 65.12% in rice plants, brown rice and rice husks, indicating a matrix-inhibitory effect, and the matrix effect was 87.06% in soils, indicating a weak matrix effect. The recovery of PBU addition was 77.61% to 100.12% in different samples, with RSD of 1.43% to 6.74%, and a limit of quantification (LOQ) of 0.005 mg/kg, and the addition recovery and RSD met the requirements of the Guidelines for Pesticide Residue Testing in Crops (NY/T 788-2018), validating the effectiveness of UPLC-MS/MS assay. Following spraying PBU at a dose of 1 kg/667 m2, the half-life of PBU was 6.24 d in rice plants and 3.43 d in paddy water samples, respectively. The final residues of PBU were lower than the LOQ of 0.005 mg/kg in brown rice and rice husk samples 98 d following spraying PBU. Following spraying PBU at a dose of 5 kg/667 m2, the half-life of PBU was 15.75 d in rice plants and 7.62 d in paddy water samples, respectively. The final residue of PBU was lower than the LOQ of 0.005 mg/kg in brown rice 98 d following spraying PBU, and the final residue of PBU was 0.049 mg/kg in rice husks.

Conclusions: A simple, and highly accurate and precise UPLC-MS/MS assay has been developed for determination of PBU residues in rice plants and paddy environments through extraction and purification of PBU from matrix samples using QuEChERS pretreatment. After spraying PBU in paddies, the concentration of PBU gradually decreases in rice plants and paddy water over time, and the final residual concentration is low.

求助全文
通过发布文献求助,成功后即可免费获取论文全文。 去求助
来源期刊
中国血吸虫病防治杂志
中国血吸虫病防治杂志 Medicine-Medicine (all)
CiteScore
1.30
自引率
0.00%
发文量
7021
期刊介绍: Chinese Journal of Schistosomiasis Control (ISSN: 1005-6661, CN: 32-1374/R), founded in 1989, is a technical and scientific journal under the supervision of Jiangsu Provincial Health Commission and organised by Jiangsu Institute of Schistosomiasis Control. It is a scientific and technical journal under the supervision of Jiangsu Provincial Health Commission and sponsored by Jiangsu Institute of Schistosomiasis Prevention and Control. The journal carries out the policy of prevention-oriented, control-oriented, nationwide and grassroots, adheres to the tenet of scientific research service for the prevention and treatment of schistosomiasis and other parasitic diseases, and mainly publishes academic papers reflecting the latest achievements and dynamics of prevention and treatment of schistosomiasis and other parasitic diseases, scientific research and management, etc. The main columns are Guest Contributions, Experts‘ Commentary, Experts’ Perspectives, Experts' Forums, Theses, Prevention and Treatment Research, Experimental Research, The main columns include Guest Contributions, Expert Commentaries, Expert Perspectives, Expert Forums, Treatises, Prevention and Control Studies, Experimental Studies, Clinical Studies, Prevention and Control Experiences, Prevention and Control Management, Reviews, Case Reports, and Information, etc. The journal is a useful reference material for the professional and technical personnel of schistosomiasis and parasitic disease prevention and control research, management workers, and teachers and students of medical schools.    The journal is now included in important domestic databases, such as Chinese Core List (8th edition), China Science Citation Database (Core Edition), China Science and Technology Core Journals (Statistical Source Journals), and is also included in MEDLINE/PubMed, Scopus, EBSCO, Chemical Abstract, Embase, Zoological Record, JSTChina, Ulrichsweb, Western Pacific Region Index Medicus, CABI and other international authoritative databases.
×
引用
GB/T 7714-2015
复制
MLA
复制
APA
复制
导出至
BibTeX EndNote RefMan NoteFirst NoteExpress
×
提示
您的信息不完整,为了账户安全,请先补充。
现在去补充
×
提示
您因"违规操作"
具体请查看互助需知
我知道了
×
提示
确定
请完成安全验证×
copy
已复制链接
快去分享给好友吧!
我知道了
右上角分享
点击右上角分享
0
联系我们:info@booksci.cn Book学术提供免费学术资源搜索服务,方便国内外学者检索中英文文献。致力于提供最便捷和优质的服务体验。 Copyright © 2023 布克学术 All rights reserved.
京ICP备2023020795号-1
ghs 京公网安备 11010802042870号
Book学术文献互助
Book学术文献互助群
群 号:604180095
Book学术官方微信