摘要
建立高效溶剂萃取(HPSE)-气相色谱三重四级杆质谱法(GC-MS/MS)快速测定土壤中环酰菌胺、醚菌胺、唑嘧菌胺和萎锈灵微量残留的分析方法。随机选取土壤样品,粉碎过80目筛网,取过筛后的土壤样品约12 g,装填至萃取罐中,再用硅藻土填满,旋紧盖子,将其置于高效溶剂萃取仪(HPSE)中进行提取,提取液浓缩至近干,加1 mL丙酮溶解,涡旋1 min,0.22μm过滤后,上气相色谱质谱仪定量检测。环酰菌胺、醚菌胺、唑嘧菌胺和萎锈灵在质量浓度0.02~10.0μg/mL范围内具有良好的线性;平均加标回收率范围:91.4%~104.9%;检出限在0.010~0.022 mg/kg之间;重复性和精密度RSD均小于5%(n=6)。结果表明,该方法具有快捷、准确、环境友好等特点,适用于土壤中微量酰胺类杀菌剂残留的检测。
To establish high efficiency solvent extraction(HPSE)united Gas chromatography-triple four-step mass spectrometry(GC-MS/MS)method for rapid determination of four pesticide residuals(fenhexamid,dimoxystrobin,ametoctradin and carboxin)in soil.Random soil samples were grinded and sieved by 80 mesh first,took 12 g samples to extract pond and filled it with diatomaceous earth.Screw the lid on tightly,put the extract pond on HPSE and extracted samples.The extracted solution was flowed to near dry by nitrogen,and volumned to 1 mL by acetone.Samples were analyzed on GC-MS/MS after filtered by 0.22μm filter membrane and vortexed for 1 min.Fenhexamid,dimoxystrobin,ametoctradin and carboxin showed good linear relationships in the concentration range of 0.02 to 10.0μg/mL.Average recoveries were varied from 91.4%-104.9%.The detection limits were in the range of 0.010 to 0.022 mg/kg and Relative standard deviation(RSD)of repeatability and precision were below 5%(n=6).The results show that this method is fast,accurate and environmentally friendly,and is suitable for the detection of amide fungicides in soil.
作者
刘永玲
郭延萍
LIU Yongling;GUO Yanping(Monitoring Station of Haidong Ecological Environment Bureau,Haidong 810600,China)
出处
《中国测试》
CAS
北大核心
2021年第5期64-67,103,共5页
China Measurement & Test
