38%唑醚·啶酰菌悬浮剂在草莓和土壤中的残留及消解动态
投稿时间:2017-10-10      点此下载全文 HTML
引用本文:杨霄鸿,赵楠楠,赵文文,刘慧君,金芬,贾明宏,等.38%唑醚·啶酰菌悬浮剂在草莓和土壤中的残留及消解动态[J].农药学学报,2018,20(1):67-74.
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杨霄鸿 北京农学院 食品科学与工程学院/食品质量与安全北京实验室, 北京 102206;北京农学院 食品科学与工程学院/农产品有害微生物及农残安全检测与控制北京市重点实验室, 北京 102206  
赵楠楠 北京农学院 食品科学与工程学院/食品质量与安全北京实验室, 北京 102206;北京农学院 食品科学与工程学院/农产品有害微生物及农残安全检测与控制北京市重点实验室, 北京 102206  
赵文文 中国农业科学院 农业质量标准与检测技术研究所/农业部农产品质量安全重点实验室, 北京 100081  
刘慧君 北京农学院 食品科学与工程学院/食品质量与安全北京实验室, 北京 102206;北京农学院 食品科学与工程学院/农产品有害微生物及农残安全检测与控制北京市重点实验室, 北京 102206 huijunliu78@163.com 
金芬 中国农业科学院 农业质量标准与检测技术研究所/农业部农产品质量安全重点实验室, 北京 100081 jinfenbj@163.com 
贾明宏 北京农学院 食品科学与工程学院/食品质量与安全北京实验室, 北京 102206;北京农学院 食品科学与工程学院/农产品有害微生物及农残安全检测与控制北京市重点实验室, 北京 102206  
基金项目:北京高等学校高水平人才交叉培养“实培计划”毕业设计(科研类);国家自然科学基金(31601658)
中文摘要:为评价38%唑醚·啶酰菌悬浮剂(有效成分质量分数:12.8%吡唑醚菌酯,25.2%啶酰菌胺)在农产品和环境中的安全性,于2015年和2016年在中国北京及山东分别进行了该药剂在草莓及土壤中的残留及消解动态试验,建立了同时测定草莓及土壤中吡唑醚菌酯和啶酰菌胺残留量的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品用乙腈提取,经N-丙基乙二胺(PSA)净化,电喷雾多反应监测模式HPLC-MS/MS检测,基质匹配标准曲线外标法定量。结果表明:在草莓和土壤中添加0.015~3.0 mg/kg吡唑醚菌酯,平均回收率分别为97%~107%和94%~106%,相对标准偏差(RSD)分别为1.8%~3.9%和2.2%~4.1%,定量限(LOQ)为0.015 mg/kg;添加0.03~6.0 mg/kg啶酰菌胺,平均回收率分别为90%~101%和92%~97%,RSD为4.6%~13%和2.9%~14%,LOQ为0.03 mg/kg。田间试验结果表明,吡唑醚菌酯和啶酰菌胺在草莓和土壤中的消解动态均符合一级动力学方程,在草莓中的半衰期分别为4.8~6.0 d和5.1~11 d,在土壤中为3.4~10.0和3.4~6.0 d。采用38% 唑醚·啶酰菌悬浮剂,分别按有效成分228和342 g/hm2于草莓幼果期施药,最多施药 4 次,采样时间距离最后一次施药的间隔时间为3、5、7 d。吡唑醚菌酯在草莓中的最大残留量为 0.13 mg/kg,低于欧盟规定的最大残留限量(MRL)(0.5 mg/kg);啶酰菌胺在草莓中的最大残留量为 0.78 mg/kg,低于中国的 MRL值(3.0 mg/kg)。建议38%唑醚·啶酰菌悬浮剂在草莓上的安全间隔期为3 d,试验结果为农药在草莓中的安全使用和农产品的食用安全提供了数据支持。
中文关键词:吡唑醚菌酯  啶酰菌胺  草莓  土壤  残留  消解  高效液相色谱-串联质谱法
 
Residue and dissipation dynamics of 38% pyraclostrobin·boscalid SC in strawberry and soil
Abstract:In order to evaluate the safety of 38% pyraclostrobin·boscalid suspension concentrate (SC) (mass fraction of active ingredient: 12.8% of pyraclostrobin, 25.2% boscalid) in agricultural products and environment, the residues and dissipation dynamics of the agent were investigated in field experiments in Beijing and Shandong for two years (2015 and 2016). The residues of pyraclostrobin and boscalid simultaneously in strawberry and soil were determined by a new high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) analysis method. The samples were extracted by acetonitrile, purified by N-propyl ethylenediamine (PSA), measured by multiple reaction monitoring (MRM) using electrospray ionization and quantified via matrix matching external standard curve. At spiked levels of 0.015, 1.5 and 3.0 mg/kg, the average recoveries of pyraclostrobin in strawberry and soil samples were 97%-107% and 94%-106%, respectively, and RSDs were 1.8%-3.9% and 2.2%-4.1%, respectively. The limit of quantitation (LOQ) of pyraclostrobin in strawberry samples was 0.015 mg/kg. At spiked levels of 0.03, 3.0 and 6.0 mg/kg, the average recoveries of boscalid in strawberry and soil samples were 90%-101% and 92%-97%, respectively, and RSDs were 4.6%-13% and 2.9%-14%, respectively. The LOQ of boscalid in strawberry samples was 0.03 mg/kg. In the decline study, the dissipation equations of pyraclostrobin and boscalid in strawberry and soil samples fit the first-order kinetics equation, and the half-lives for the dissipation of these pesticides were 4.8-6.0 d and 5.1-11 d, respectively, in strawberry, while 3.4-10.0 d and 3.4-6.0 d, respectively, in soil. Following the recommended dosage of 38% pyraclostrobin o boscalid SC in strawberry (active ingredient: 228 and 342 g/hm2), the samples were applied for less than 4 times and collected 3, 5 and 7 d after the last application. The maximum final residue of pyraclostrobin in the strawberry was 0.13 mg/kg, which was below the maximum residual limit (MRL) (0.5 mg/kg) of EU. And that of boscalid was 0.78 mg/kg, which was lower than the MRL (3.0 mg/kg) of China. The safety interval of 38% pyraclostrobin. boscalid SC for strawberry is 3 days. The test results provide data support for the safe use of pesticides in strawberries and the food safety of agricultural products.
Key words:pyraclostrobin  boscalid  strawberry  soil  residue  dissipation  high performance liquid chromatography-tandem mass spectrometry
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