QuEChERS-GC-MS/MS Detetermination of Residual Amount of 6 Methoxy Acrylate Fungicides in 3 Edible Mushrooms
摘 要
本工作建立了一种QuEChERS-气相色谱-串联质谱法(GC-MS/MS)测定3种食用菌中6种甲氧基丙烯酸酯类杀菌剂(啶氧菌酯、醚菌酯、嘧螨酯、醚菌胺、吡唑醚菌酯、氟嘧菌酯)残留量的分析方法。称取25.0 g粉碎后的食用菌样品,加入体积比为1∶1的环己烷-乙酸乙酯溶液25 mL,再加入QuEChERS萃取包,涡旋后冷冻离心;将上清液转移至PSA净化管中,涡旋后离心;取上清液10 mL在60℃氮吹至近干,加入体积比为1∶1的环己烷-乙酸乙酯溶液1.0 mL,涡旋溶解后过0.22 μm滤膜,滤液引入Rtx-5 MS色谱柱,载气为氦气,在分流进样、程序升温的条件下进行色谱分离,并在电子轰击离子源(EI)和多反应监测(MRM)模式下进行质谱分析,采用外标法定量。6种甲氧基丙烯酸酯类杀菌剂在0.02~2.0 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)为0.001~0.003 mg·kg-1;对香菇、鸡腿菇和金针菇等3种常见食用菌进行3个浓度水平的加标回收试验,测得回收率为83.5%~105%,测定值的相对标准偏差(n=6)为1.7%~5.0%,重复性RSD在5.0%以内。
Abstract
An analytical method for determination of 6 methoxy acrylate fungicides (picoxystrobin, kresoxim-methyl, fluacrypyrim, dimoxystrobin, pyraclostrobin and fluoxastrobin) in the 3 edible mushrooms by QuEChERS-GC-MS/MS was established in the work. 25.0 g of the crushed edible mushrooms samples were taken, and mixed with by 25 mL of cyclohexane-ethyl acetate solution at a volume ratio of 1:1 to extract the 6 fungicides by shaking. The mixture was vortexed and freeze-centrifuged after adding the QuEChERS extraction package. The extracted solution was then transferred to PSA purification tube. After vortexing and centrifuging, 10 mL of the supernatant was taken and evaporated to near-dryness by N2-blowing at 60℃. 1 mL of cyclohexane-ethyl acetate solution at a volume ratio of 1:1 was added to the residue, and the mixture was dissolved by swirling, and filtered through 0.22 μm filter membrane. The filtrate was introduced to Rtx-5 MS chromatographic column and separated under the condition of split-flow sample introduction and programmed temperature elevation with helium gas as carrier, and then analyzed by MS/MS with EI and MRM mode. External standard method was used in quantitative analysis. Linearity relationships between values of mass fraction of the 6 fungicides and its respective peak areas were found in the same range of 0.02-2.0 mg·L-1, with detection limits (3S/N) of 0.001-0.003 mg·kg-1. Test for the spiked recovery were made at 3 concentritions for the 3 edible mushrooms such as shiitake mushrooms, coprinus comatus and enoki mushrooms, giving results of recovery ranged from 83.5% to 105%. Values of RSDs (n=6) found were in the range of 1.7%-5.0%, with RSDs (n=6) of repeatibility less than 5.0%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202006006
所属栏目 工作简报
基金项目 福建省自然科学基金(2019J01734);广西高校中青年教师科研基础能力提升项目(2020KY06038);广西自然科学基金联合资助培育项目(2019GXNSFAA245058);广西自然科学基金(2017GXNSFAA198186)
收稿日期 2019/12/2
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备注范良彪,助理实验师,硕士,从事实验室管理和分析工作
引用该论文: FAN Liangbiao,WU Qingshi,HUANG Lili,HUANG Yuequn,LIANG Meina,ZHANG Qing. QuEChERS-GC-MS/MS Detetermination of Residual Amount of 6 Methoxy Acrylate Fungicides in 3 Edible Mushrooms[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(6): 655~660
范良彪,吴清实,黄丽丽,黄月群,梁美娜,张庆. QuEChERS-气相色谱-串联质谱法测定3种食用菌中6种甲氧基丙烯酸酯类杀菌剂的残留量[J]. 理化检验-化学分册, 2020, 56(6): 655~660
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【3】冯彦媚,范兴辉,占卉,等.甲氧基丙烯酸酯类农药生态毒理及其微生物降解研究进展[J].生物技术通报, 2017(10):52-58.
【4】张一宾.甲氧基丙烯酸酯类杀菌剂的全球市场概况及进展[J].世界农药, 2016,38(4):30-34.
【5】张金霞,陈强,黄晨阳,等.食用菌产业发展历史、现状与趋势[J].菌物学报, 2015,34(4):524-540.
【6】张丹,袁雅文.气相色谱串联质谱法测定食用菌中拟除虫菊酯类农药[J].河南预防医学杂志, 2019,30(7):508-511.
【7】柏亚罗.嘧菌酯、吡唑醚菌酯等六大产品以绝对优势统领甲氧基丙烯酸酯类杀菌剂市场[J].山东农药信息, 2018(4):24-30.
【8】吴洁珊,冯家望,任永霞,等.气相色谱测定柑橘中多种甲氧基丙烯酸酯类杀菌剂的残留量[J].农药, 2011,50(10):754-755.
【9】周瑶,杨惠琴,时逸吟,等.超高效液相色谱-串联质谱法检测水果中6种甲氧基丙烯酸酯类杀菌剂及其质谱裂解规律[J].色谱, 2017,35(9):970-979.
【10】张婷,彭红,金鑫,等.高效液相色谱法测定对氯苯氧异丁酸甲氧基苯丙烯酸酯胶囊含量及有关物质[J].中国新药杂志, 2016,25(24):2854-2861.
【11】赵光骞,雷国明,赵显正,等.固相萃取-GC-MS/MS检测饮用水中常见的8种农残物[J].食品工业, 2018,39(12):273-276.
【12】王慎苓,于丽,李安荣,等.QuEChERS方法在果蔬农药多残留检测中的应用[J].食品与药品, 2019,21(3):231-234.
【13】徐纬,刘天洁,黄琴.蔬菜中五氯硝基苯和百菌清残留测定的QuEChERS应用与优化[J].贵州医科大学学报, 2019,44(7):810-813.
【14】林捷,张彩云,柯华,等.花草茶中11种杀菌剂QuEChERS-超高效液相色谱-串联质谱快速测定法[J].职业与健康, 2019,35(6):748-751.
【15】崔丽丽,闫梅霞,朴向民,等.QuEChERS-气相色谱-质谱联用法快速测定人参中农药多残留[J].色谱, 2018,36(11):1173-1180.
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