壬菌铜和吡唑醚菌酯在苹果和土壤中的残留及消解动态

发布时间：2018-03-24 13:00

本文选题：壬菌铜　切入点：吡唑醚菌酯　出处：《农药学学报》2017年01期

【摘要】：建立了同时测定苹果及其土壤中壬菌铜和吡唑醚菌酯残留的分散固相萃取-高效液相色谱-串联质谱(DSPE-HPLC-MS/MS)方法,并采用该方法研究了24%吡唑醚菌酯·壬菌铜微乳剂在苹果和土壤中的残留及消解动态。其中壬菌铜以硫化钠为破络剂,将其转化为壬基酚磺酸后进行检测。样品用乙腈提取,同时加入硫化钠,经N-丙基乙二胺(PSA)净化后,采用C_(18)色谱柱,以甲醇-水为流动相梯度洗脱分离,于多反应监测模式下经正负离子同时扫描进行定性,基质匹配标准曲线外标法定量。结果表明:在0.1~10 mg/kg添加水平下,壬菌铜在苹果及土壤中的回收率范围为92%~103%,相对标准偏差(RSD)为1.3%~5.1%;在0.01~1 mg/kg添加水平下,吡唑醚菌酯在苹果及土壤中的回收率范围为96%~105%,RSD为2.4%~4.6%。苹果及土壤中壬菌铜和吡唑醚菌酯的最低检测浓度(LOQ)分别为0.1和0.01 mg/kg。2014 2015年,中国宁夏、北京和山东两年三地的田间残留试验表明:壬菌铜在苹果和土壤中的消解半衰期分别为2.7~5.4和2.0~5.8 d,吡唑醚菌酯在苹果和土壤中的消解半衰期分别为4.3~8.3和3.6~10.2 d;采用24%吡唑醚菌酯·壬菌铜微乳剂,分别按推荐剂量(有效成分300 mg/kg)和推荐剂量的1.5倍(有效成分450 mg/kg)于苹果幼果期施药,最多施药4次,距末次施药14 d时,壬菌铜在苹果中的最大残留量为0.31 mg/kg,远低于日本规定的最大允许残留限量(MRL)值(5 mg/kg),吡唑醚菌酯在苹果中的最大残留量为0.27 mg/kg,低于中国规定的MRL值(0.5 mg/kg)。
[Abstract]:A DSPE-HPLC-MS / MS / MS method for simultaneous determination of copper and pyrazolyl ester residues in apple and its soil was established by DSPE-HPLC-MS / MS. This method was used to study the residue and digestion dynamics of 24% pyrazolyl nonylazolyl nonylphenol copper microemulsion in apple and soil. Nonylphenol sulfonic acid was transformed into nonylphenol sulfonic acid, and the sample was extracted with acetonitrile. At the same time, sodium sulfide was added, purified by N-propylethylenediamine (PSA), and then chromatographic column was used as C _ S _ (18) column. The mobile phase gradient elution was carried out with methanol-water, and the qualitative analysis was carried out by simultaneous positive and negative ion scanning under the multi-reaction monitoring mode. The results showed that the recovery rate of nonylenium copper in apple and soil was 922 ~ 103 and the relative standard deviation (RSD) was 1.3 ~ 5.1cm under 0.1 ~ 10 mg/kg addition level, and at 0.01 ~ (-1) mg/kg level, the relative standard deviation was 1.31%. The recoveries of pyrazole in apple and soil were 96 ~ 105RSD = 2.4 and 4.6.The lowest detectable concentrations of nonylated copper and pyrazole in apple and soil were 0. 1 and 0. 01 mg/kg.2014 respectively. The field residue experiments in Beijing and Shandong showed that the half-life of nonylated copper in apple and soil was 2.74.4,2.058.days, and the half-life of pyrazole in apple and soil was 4.38.3,3.610.2 days, and 24% in apple and soil, respectively. Copper microemulsion of nonyl nonyl Ester of Pyrazole Ether, The recommended dose (300 mg / kg of active ingredient) and 1.5 times of recommended dose (450 mg / kg of active ingredient) were applied at the young fruit stage of apple at most 4 times, 14 days after the last application. The maximum residual amount of nonylenium copper in apple was 0.31 mg / kg, which was much lower than the maximum allowable residue limit (MRL) of 5 mg / kg in Japan, and the maximum residual amount of pyrazole in apple was 0.27 mg / kg, which was lower than the MRL value of 0.5 mg / kg specified by China.
【作者单位】：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;
【基金】：国家自然科学基金(31401590)
【分类号】：S481.8;O657.63

【参考文献】