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QuEChERS样品制备系统联合气相色谱-串联质谱法测定松林土壤中6种杀虫剂的残留量
          
Determination of Residues of 6 Insecticides by Gas Chromagraphy-Tandem Mass Spectrometry Combined with QuEChERS Sample Preparation System

摘    要
随机采集松林土壤样品,风干、除杂、粉碎、过筛,分取10 g置于QuEChERS样品制备系统整合管外管中,加入一个氧化锆瓷珠包(20粒氧化锆瓷珠)、20 mL乙腈和一个QuEChERS提取包(内置5.0 g无水硫酸镁和1.0 g乙酸钠),再将内置1.0 g无水硫酸镁、500 mg N-丙基乙二胺(PSA)、500 mg C18和15 mg石墨化碳黑(GCB)的一个QuEChERS净化包置于整合管内管中,将整合管加载至QuEChERS样品制备系统,振荡10 min,离心5 min,重复上述振荡和离心过程一次,即完成样品的提取和净化。收集净化液,冷冻离心5 min,上清液于50℃氮吹至近干,残渣用1 mL丙酮复溶,过0.22 μm滤膜,滤液供气相色谱-串联质谱法(GC-MS/MS)分析。6种杀虫剂(氯氟氰虫酰胺、氰戊菊酯、戊菊酯、治线磷、丰索磷和杀螟松)用Rxi-5Sil MS色谱柱在程序升温条件下分离,用电子轰击离子(EI)源电离,用多反应监测(MRM)模式检测,外标法定量。结果显示:6种杀虫剂的质量浓度在0.01~3.00 mg·L-1内与峰面积呈线性关系,检出限(3S/N)为0.012~0.021 μg·kg-1;按照标准加入法进行回收试验,回收率为86.2%~102%,测定值的相对标准偏差(n=5)为1.6%~4.2%;方法用于5份实际样品的分析,检出了丰索磷、杀螟松、氰戊菊酯和氯氟氰虫酰胺,检出量为14.22~125.35 μg·kg-1
标    签 QuEChERS样品制备系统   气相色谱-串联质谱法(GC-MS/MS)   松林土壤   杀虫剂   残留量   QuEChERS sample preparation system   gas chromatography-tandem mass spectrometry (GC-MS/MS)   pine forest soil   insecticide   residue  
 
Abstract
Pine forest soil samples were randomly collected, dried by air, removed impurities, ground and sieved. An aliquot (10 g) of the sample together with a zirconia ceramic bead bag (20 zirconia ceramic beads), 20 mL of acetonitrile and a QuEChERS extraction bag (containing 5.0 g of anhydrous magnesium sulfate and 1.0 g of sodium acetate) was taken and placed into the outer tube of the QuEChERS sample preparation system integration tube. A QuEChERS purification bag containing 1.0 g of anhydrous magnesium sulfate, 500 mg of PSA, 500 mg of C18 and 15 mg of GCB was placed into the inner tube of the integration tube, and the integration tube was loaded into the QuEChERS sample preparation system. The mixture was shaken for 10 min and centrifuged for 5 min, and the above shaking and centrifugation processes were repeated once, to complete the extraction and purification of the sample. The purified solution was collected, and freeze centrifuged for 5 min. The supernatant was blown to near dryness at 50℃ by nitrogen, and the residue was dissolved by 1 mL of acetone. The resulting solution was passed through a 0.22 μm filter membrane, and the filtrate was analyzed by GC-MS/MS. Six insecticides (cyhalodiamide, fenvalerate, valerate, curmidophos, fensulfothion and fenitrothion) were separated by Rxi-5Sil MS column under temperature programmed conditions, ionized by EI source, detected by MRM mode, and quantified by external standard method. It was shown that linear relationships between values of the mass concentration and the peak area of the 6 insecticides were kept in the range of 0.01-3.00 mg·L-1, with detection limits (3S/N) in the range of 0.012-0.021 μg·kg-1. Test for recovery was made according to standard addition method, giving recoveries in the range of 86.2%-102%, and RSDs (n=5) of the determined values ranged from 1.6% to 4.2%. The proposed method was applied to the analysis of 5 actual samples, and fensulfothion, fenitrothion, fenvalerate and cyhalodiamide were detected, with detection amounts in the range of 14.22-125.35 μg·kg-1.

中图分类号 O657.63   DOI 10.11973/lhjy-hx202308014

 
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收稿日期 2022/2/4

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备注丁波涛,高级工程师,主要从事环境监测工作,253361688@qq.com

引用该论文: DING Botao,WANG Suhua,GUO Liang,WANG Binghui,LIU Dawei. Determination of Residues of 6 Insecticides by Gas Chromagraphy-Tandem Mass Spectrometry Combined with QuEChERS Sample Preparation System[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(8): 953~957
丁波涛,王素华,郭亮,王丙晖,刘大卫. QuEChERS样品制备系统联合气相色谱-串联质谱法测定松林土壤中6种杀虫剂的残留量[J]. 理化检验-化学分册, 2023, 59(8): 953~957


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参考文献
【1】孟祥江,何邦亮,马正锐,等.我国马尾松林经营现状及近自然育林探索[J].世界林业研究, 2018,31(3):63-67.
 
【2】潘金勇,韦家欣.不同整地方式对马尾松造林成活率的影响[J].林业科技情报, 2016,48(3):38-39.
 
【3】罗应华,孙冬婧,林建勇,等.马尾松人工林近自然化改造对植物自然更新及物种多样性的影响[J].生态学报, 2013,33(19):6154-6162.
 
【4】范立淳,时勇,姜生伟,等.辽宁携带松材线虫的天牛种类研究[J].林业科学研究, 2021,34(6):174-181.
 
【5】程飞侠.绩溪县松材线虫疫区大面积枯死松树清理方法及对策建议[J].安徽农学通报, 2021,27(22):88-89.
 
【6】李洋,郝昕,李明锐,等.松材线虫P糖蛋白在药物代谢过程中的功能研究[J].北京林业大学学报, 2021,43(11):71-78.
 
【7】刘长霞.浅析松材线虫的防治与处理[J].新农业, 2018(17):31-32.
 
【8】陈根林.松树化学分类与松材线虫病抗性研究[J].安徽林业科技, 2021,47(5):7-10.
 
【9】韩玲玲,乔龙.泗水县松材线虫病发生及其综合防治技术[J].陕西林业科技, 2021,49(5):128-130.
 
【10】熊彩云,涂业苟,刘晓华,等.氯氟氰虫酰胺对松材线虫的毒力测定[J].南方林业科学, 2020,48(4):66-70.
 
【11】罗钰.固相萃取-GC-ECD法检测土壤中的腐霉利、氰戊菊酯、甲氰菊酯和五氯硝基苯残留量[J].化学工程师, 2020,34(8):28-30.
 
【12】蔡邦成,赵胜豪,张卫东.加速溶剂萃取-GC-MS/MS法测定杨梅种植土壤中5种菊酯类农药[J].食品工业, 2020,41(5):307-309.
 
【13】黄美玲,林毅楠,周杨,等.液相色谱串联质谱法测定油料作物中3种双酰胺类杀虫剂残留量[J].食品安全质量检测学报, 2020,11(15):5099-5106.
 
【14】杨春霞,卫平萍,余明池.QuEChERS-UPLC法测定水果中三氯杀螨醇和氰戊菊酯残留量[J].安徽预防医学杂志, 2021,27(1):78-80.
 
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