气相色谱串联质谱法同时测定土壤样品中5种含溴类农药  

Simultaneous determination of five brominated pesticides in soil samples by GC-MS/MS

作　　者：赵光骞 李海景 赵海军 ZHAO Guang-qian;LI Hai-jing;ZHAO Hai-jun(Nanyang Ecological Environment Monitoring Center in Henan Province,Nanyang 473000,China;Tongbai Branch of Nanyang Ecological Environment Bureau,Nanyang 474750,China;Henan Province South to North Water Diversion Canal Head Ecological Environment Monitoring Emergency Center,Nanyang 474475,China)

机构地区：[1]河南省南阳生态环境监测中心,河南南阳473000 [2]南阳市生态环境局桐柏分局,河南南阳474750 [3]河南省南水北调渠首生态环境监测应急中心,河南南阳474475

出　　处：《化学研究与应用》2024年第9期2164-2168,共5页Chemical Research and Application

摘　　要：研究建立了QuEChERS提取、净化土壤样品中5种含溴类农药(溴丁酰草胺、乙基溴硫磷、溴苯烯磷、氯溴隆和辛酰溴苯睛)的气相色谱-三重四级杆串联质谱定量测定的分析方法。称取10g预处理后的土壤样品到QuEChERS样品管中,分别加人20mL乙睛,1颗陶瓷均质子,QuEChERS提取包(含有6gMgSO_(4),1.5g醋酸钠),将装有净化剂(1g的MgSO_(4),150mg的PSA和15mg的CCB)的内管置于整合管中,以8000r·min^(-1)的速率离心5分钟进行提取、净化。取净化液2mL氮吹至近干,加1mL溶剂溶解,滤过后,上机检测,外标法定量。5种含溴类农药在0.005~0.5μg·mL^(-1)范围内线性良好,R^(2)均大于0.995;检测限依次为:溴丁酰草胺:0.013mg·kg^(-1),氯溴隆:0.010mg·kg^(-1),乙基溴硫磷:0.011mg·kg^(-1),溴苯烯磷:0.008mg·kg^(-1),辛酰溴苯睛:0.015mg·kg^(-1)。三水平回收率在89.3%~110.5%之间。该方法自动化程度高、溶剂使用量少,可用于土壤中含溴类农药残留的监测。To establish QuEChERS extraction and purification method for quantitative determination of five bromo-containing pesticides(bromobutide,Rilariol,bromo fenetho phosphorion,chlorbromuron and octyl bromobenzitrile)in soil samples by gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS).Pretreated 10 g of soil samples was took into QuEChERS sample tubes,20 mL acetonitrile and 1 ceramic homonitrile were added,respectively.QuEChERS extraction pack(containing 6g MgSO_(4) and 1.5g sodium acetate),inner tubes containing purifiers(1g MgSO_(4),150mg PSA and 15mg GCB)were placed in the integrator tube,and QuEChERS pre-treatment equipment parameters were set.Centrifugation was performed at a rate of 8000 r·min^(-1) for 5 min for extraction and purification.2mL purified solution were took and blowed to nearly dry by nitrogen.Residues was fixed to lmL with ethyl acetate,After filtration by 0.22um filter,the samples were separated by Rtx-5 column(30 m×250μm,0.25μm),analyzed by GC-MS/MS and quantified by external standard method.The five bromo-containing highly toxic pesticides had good linear relationships in the concentration range of 0.005~0.5μg·mL^(-1),with correlation coefficients all above 0.995.Detection limits were as follows:bromobutide:0.013 mg·kg,Rilariol:0.010 mg·kg^(-1),bromo fenetho phosphorion:0.011 mg·kg^(-1),chlorbromuron:0.008 mg·kg^(-1),octyl bromobenzitrile:0.015 mg·kg^(-1).Average recoveries were ranged from 89.3%to 110.5%.Relative standard deviation(RSD)of precision were within 5%(n=6).The method has high automation and less solvent,and can be used to monitor the residues of bromine pesticides in soil.

关 键 词：QUECHERS GC-MS/MS 土壤 含溴类农药 溴丁酰草胺 

分 类 号：O657.7[理学—分析化学]