加速溶剂萃取-多壁碳纳米管净化联合UPLC-MS/MS检测橘类水果栽培土壤中六种农药残留  

Accelerated solvent extraction-multi wall carbon nanotube purification combined with UPLC-MS/MS to detect residues of pesticide in orange fruit cultivation soil

作　　者：蒋幸幸 JIANG Xing-xing(Henan Nanyang Ecological Environment Monitoring Center,Nanyang 473000,China)

机构地区：[1]河南省南阳生态环境监测中心,河南南阳473000

出　　处：《化学研究与应用》2024年第11期2490-2496,共7页Chemical Research and Application

摘　　要：实验建立加速溶剂萃取-多壁碳纳米管净化联合UPLC-MS/MS检测橘类水果栽培土壤中苯菌灵、多菌灵、噻菌铜、咪鲜胺、嘧菌酯和百菌清农药残留的分析方法。取橘类水果栽培土壤500g,风干、粉碎、过筛;准确称取过筛网后的样品12g,置加速溶剂萃取池中,再加20g硅藻土,用25mL乙醇-乙酸乙酯(V:V=1:1)提取;提取液置烧杯中,静置30min后,吸取上清液5mL,置25mL离心管中,再加入10mg多壁碳纳米管和200mg无水硫酸镁,涡旋2min使之充分混匀,以10000r·min^(-1)速度离心5min;取出离心管,将上清液过滤,续滤液作为样品溶液,上UPLC-MS/MS仪定性、定量检测。苯菌灵、多菌灵、噻菌铜、咪鲜胺、嘧菌酯和百菌清6种农药在0.001~5.0mg·L^(-1)范围内具有良好的线性,相关系数(r)均大于0.995;检测限分别为0.004、0.003、0.008、0.0050.007和0.002μg·L^(-1)三水平加标回收率均在84.4~103.1%之间。实验证明此方法具有准确、快速等优点,可以用于橘类水果栽培土壤中苯菌灵、多菌灵、噻菌铜、咪鲜胺、嘧菌酯和百菌清等常用农药的检测。To establish an accelerated solvent extraction(ASE)-multi wall carbon nanotube purification combined with Ultra Performance Liquid Chromatography Mass Spectrum(UPLC-MS/MS)to detect residues of benomyl,carbendazim,thiazepam,prochloraz,azoxystrobin and chlorothalonil in orange fruit cultivation soil.500 g of orange fruit cultivation soil were taken,air dried,crushed and sifted.12 g of the pretreated sample were accurately weighed and placed in an accelerated solvent extraction tank.20 g diatomite were added,samples were extracted with 25 mL ethanol-ethyl acetate(V:V=1:1).The extraction solution was placed in a beaker for 30 min,then 5 mL of the supernatant was absorbed and placed in a 25 mL centrifuge tube.10 mg of multi-walled carbon nanotubes and 200 mg of anhydrous magnesium sulfate were added and vortexed for 2 min to mix thoroughly,then centrifuge at a speed of 10000r·min^(-1)for 5 min.The supernatant were filtered and use the furtherfiltrate as the sample solution for qualitative and quantitative detection on the UPLC-MS/MS instrument.Benomyl,carbendazim,thiazepam,prochloraz,azoxystrobin and chlorothalonil showed good linear relationships in the concentration ranges of 0.001~5.0 mg·L^(-1),with correlation coefficients(r)all greater than 0.995.Detection limits were 0.004μg·L^(-1)、0.003μg·L-0.008μg·L^(-1)、0.005μg·L^(-1)、0.007μg·L^(-1)and 0.002μg·L^(-1),respectively.Average recoveries in 3 concentration levels were 84.4~103.3%.The experimental results showed that the method was accurate and rapid,and could be used for the detection of benzodiazepam,carbendazim,thiazepam,midazepam,pyrimidon and chlorothalonil in the soil of orange fruit cultivation.

关 键 词：加速溶剂萃取 多壁碳纳米管 土壤 农药 

分 类 号：O657.7[理学—分析化学]