摘要
[目的]基于经典的QuEChERS前处理方法,结合高效液相色谱串联质谱(HPLC-MS/MS)建立啶酰菌胺在向日葵及土壤中残留分析方法,明确啶酰菌胺在向日葵和土壤中的消解行为和最终残留。[方法]向日葵籽粒、籽粒仁和土壤经乙腈-水提取,向日葵植株经乙腈提取,经C18、PSA、GCB和无水硫酸镁净化,以0.1%甲酸水溶液-乙腈为流动相进行梯度洗脱,外标法定量,液相色谱三重四极杆质谱分析检测。[结果]啶酰菌胺在向日葵植株、向日葵籽粒、籽粒仁和土壤中0.001~1.0 mg/L质量浓度范围内色谱峰面积与质量浓度呈现良好线性;在添加水平0.01~1.0 mg/kg下,向日葵籽粒、籽粒仁和土壤中的啶酰菌胺平均回收率均处于82.5%~118.1%之间,相对标准偏差处于0.05%~5.01%之间;在添加水平0.01~15.0 mg/kg下,向日葵植株中的啶酰菌胺平均回收率处于90.6%~107.1%之间,相对标准偏差处于2.90%~6.63%之间。啶酰菌胺的定量限(LOQ)为0.01 mg/kg。啶酰菌胺在向日葵和土壤中的消解动态符合一级动力学方程,半衰期分别为1.7~3.0、5.5~8.3 d;啶酰菌胺在向日葵植株、向日葵籽粒、籽粒仁和土壤中的最终残留量分别为0.325~0.962、<0.01~0.899、<0.01~0.575、<0.01~0.447 mg/kg。[结论]该方法简单、快速、可靠,符合农药残留分析要求,适用于向日葵中啶酰菌胺残留量的检测,为向日葵中其他农药的残留检测方法提供参考。结果为指导啶酰菌胺在向日葵上的合理使用及其最大残留限量的制定提供数据支撑。
[Aims]Based on the classic QuEChERS pretreatment method combined with high-performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS),a residue analysis method for boscalid in sunflowers and soil was established to clarify its degradation behavior and final residue.[Methods]Sunflower seeds,kernels and soil were extracted with acetonitrile-water,and sunflower plants were extracted with acetonitrile.The extracts were purified with Cis,PSA,GCB and anhydrous magnesium sulfate.Gradient elution was performed with 0.1%formic acid aqueous solution-acetonitrile as mobile phase,and quantitative analysis was performed using external standard method.Liquid chromatography-triple quadrupole mass spectrometry was used for detection.[Results]The chromatographic peak area and mass concentration of boscalid showed good linearity within the concentration range of 0.001-1.0 mg/L in sunflower plants,sunflower seeds,seed kernels and soil;At the addition level of 0.01-1.0 mg/kg,the average recovery rate of boscalid in sunflower seeds,kernels and soil was between 82.5%-118.1%,with a relative standard deviation between 0.05%-5.01%;At the addition level of 0.01-15.0 mg/kg,the average recovery rate of boscalid in sunflower plants ranged from 90.6%to 107.1%,and the relative standard deviation ranged from 2.90%to 6.63%.The limit of quantification(LOQ)for boscalid was 0.01 mg/kg.The degradation dynamics of boscalid in sunflowers and soil followed a first-order kinetic equation,with half lives of 1.7-3.0 and 5.5-8.3 d,respectively;The final residual levels of boscalid in sunflower plants,sunflower seeds,seed kernels and soil were 0.325-0.962,<0.01-0.899,<0.01-0.575 and<0.01-0.447 mg/kg,respectively.[Conclusions]This method is simple,fast,reliable,and meets the requirements of pesticide residue analysis.It is suitable for the detection of boscalid residue in sunflowers and provides a reference for the detection of other pesticide residues in sunflowers.The results of this article provide data support for the rational use of boscalid on sunflowers and the establishment of its maximum residuelimit.
作者
吕佳旭
姜喜龙
熊阳
李世聪
李佳南
王丽娜
张富铭
高杉杉
刘悦
侯志广
逯忠斌
LYU Jiaxu;JIANG Xiong;XIONG Yang;LI Shicong;LI Jianan;WANG Lina;ZHANG Fuming;GAO Shanshan;LIU Yue;HOU Zhiguang;LU Zhongbin(College of Plant Protection,Jilin Agricultural University,Changchun 130118,China)
出处
《农药》
北大核心
2025年第5期342-349,353,共9页
Agrochemicals
基金
农业部行业标准制定嘧菌环胺在人参中的残留限量标准(14202008)项目资助。
