农药学学报2017，Vol.19Issue(1)：76-83,8.DOI:10.16801/j.issn.1008-7303.2017.0011
壬菌铜和吡唑醚菌酯在苹果和土壤中的残留及消解动态
Determination and dissipation dynamics of cuppric nonyl phenolsulfonate and pyraclostrobin in apples and soil
摘要
Abstract
A rapid analytical method for simultaneous determination of cuppric nonyl phenolsulfonate and pyraclostrobin in apples and soil was developed using dispersive solid phase extraction and high performance liquid chromatography-tandem mass spectrometry (DSPE-HPLC-MS/MS). Residues and dissipation of cuppric nonyl phenolsulfonate and pyraclostrobin in apples and soil were investigated. Cuppric nonyl phenolsulfonate was transformed into nonyl phenol sulfonic acid by using sodium sulfide as the complex-breaking agent. Samples were extracted by acetonitrile with the addition of sodium sulfide and then cleaned up by primary secondary amine(PSA), followed by separation on a reversed phase C18 column using methol-water as mobile phase with a gradient elution program. Qualitative and quantitative analyses were performed with electrospray ionization in both negative and positive ion modes under multiple reaction monitoring (MRM) mode. The results showed that the recoveries of cuppric nonyl phenolsulfonate at the spiked level of 0.1-10 mg/kg in apple and soil samples were in the range of 92%~103%, with relative standard deviation of 1.3%-5.1%; the recoveries of pyraclostrobin at spiked level of 0.01-1 mg/kg in apple and soil samples were in the range of 96%-105%, with relative standard deviation of 2.4%-4.6%; the limits of quantification (LOQs) of cuppric nonyl phenolsulfonate and pyraclostrobin in apple and soil samples were 0.1mg/kg and 0.01 mg/kg, respectively. Field experiments carried out in Ningxia, Shandong and Beijing during 2014–2015 showed that the half-lives of cuppric nonyl phenolsulfonate were 2.7-5.4 d in apples and 2.0-5.8 d in soil, and half-lives of pyraclostrobin were 4.3-8.3 d in apples and 3.6-10.2 d in soil. When the recommended dosage and 1.5 times of the recommended dosage (300 mg/kg and 450 mg/kg) of cuppric nonyl phenolsulfonate and pyraclostrobin (21% ME) were sprayed for 3-4 times at the young fruit period, the maximum residual concentration of cuppric nonyl phenolsulfonate and pyraclostrobin in apples with an harvest interval of 14 days was 0.31mg/kg and 0.27 mg/kg respectively, which were below the maximum residue limits (MRL) in apples for cuppric nonyl phenolsulfonate defined by Japan (5 mg/kg) and the MRL for pyraclostrobin in apple defined by China (0.5 mg/kg).关键词
壬菌铜/吡唑醚菌酯/苹果/残留/消解动态/高效液相色谱-串联质谱法/分散固相萃取Key words
cuppric nonyl phenolsulfonate/pyraclostrobin/apples/residue/dissipation/HPLC-MS/MS/dispersive solid phase extraction分类
农业科技引用本文复制引用
戚燕,杜鹏飞,张悦,王珊珊,金茂俊,王静..壬菌铜和吡唑醚菌酯在苹果和土壤中的残留及消解动态[J].农药学学报,2017,19(1):76-83,8.基金项目
国家自然科学基金 (31401590). （31401590）
