PDF《液相色谱–质谱联用测定咖啡中肟菌酯及 代谢物残留》

? 张蕊,?邓露晴,?李祥英,?等.

?液相色谱C质谱联用测定咖啡中肟菌酯及代谢物残留[J].?华南农业大学学报,?2019,?40(1):?72-76. ZHANG?Rui,?DENG?Luqing,?LI?Xiangying,?et?al.?Determination?of?trifloxystrobin?and?its?metabolite?in?coffee?by?liquid?chromatography-mass?spectrometry[J]. Journal?of?South?China?Agricultural?University,?2019,?40(1):?72-76. 液相色谱C质谱联用测定咖啡中肟菌酯及 代谢物残留 张蕊,邓露晴,李祥英,赵俊龙,李梓琳,凡帅,刘承兰 (天然农药与化学生物学教育部重点实验室/广东省生物农药创制与应用重点实验室/ 华南农业大学?农学院,广东?广州?510642) 摘要: 【目的】建立一种同时测定咖啡中肟菌酯及其代谢物肟菌酸残留量的液相色谱C质谱检测方法.【方法】样品中 待测农药组分采用含 φ 为1% 乙酸的乙腈匀浆后超声提取,氯化钠和无水硫酸镁盐析及高速离心后,取上清液经 C18 分散固相萃取净化,采用液相色谱C质谱联用检测,ESI?(+) 电离和多反应监测 (MRM) 定量测定.【结果】添加肟 菌酯质量分数为 0.01~2.00?mg・kgC1 时,肟菌酯在咖啡全果中的添加回收率为 87.8%~106.7%,相对标准偏差 (RSD) 为1.3%~5.8%;

在咖啡豆中添加回收率为 83.2%~88.1%,RSD 为2.0%~6.2%.肟菌酸在咖啡全果中的添加回 收率为 71.5%~106.0%,RSD 为1.0%~6.1%;

在咖啡豆中的添加回收率为 84.4%~105.2%,RSD 为1.0%~5.2%.肟菌 酯及肟菌酸在咖啡中的最小检出量均为 2.5*10C12 ?g,最低检出限均为 0.01?mg・kgC1 .【结论】该方法操作简便、快速 和稳定,可以满足咖啡实际样品中肟菌酯及其代谢物肟菌酸的残留检测要求. 关键词: 肟菌酯;

肟菌酸;

液相色谱C质谱联用;

农药残留;

咖啡 中图分类号: S482.2? ?文献标志码: A ?文章编号: 1001-411X(2019)01-0072-05 Determination of trifloxystrobin and its metabolite in coffee by liquid chromatography-mass spectrometry ZHANG?Rui,?DENG?Luqing,?LI?Xiangying,?ZHAO?Junlong,?LI?Zilin,?FAN?Shuai,?LIU?Chenglan (Key?Laboratory?of?Natural?Pesticide?and?Chemical?Biology,?Ministry?of?Education/Key?Laboratory?of?Bio-pesticide Innovation?and?Application?of?Guangdong?Province/College?of?Agriculture,?South?China?Agricultural University,?Guangzhou?510642,?China) Abstract: 【Objective】To?develop?a?method?for?determining?trifloxystrobin?and?its?metabolite?trifloxystrobin acid?simultaneously?in?coffee?by?liquid?chromatography-mass?spectrometry?(LC-MS).【Method】The?sample was?ultrasonically?extracted?with?acetonitrile?(including?φ=1%?acetic?acid),?and?salted?out?with?sodium?chloride and?anhydrous?magnesium?sulfate.?After?high-speed?centrifugation,?the?supernatant?was?purified?by?C18 dispersive?solid-phase?extraction?and?detected?by?LC-MS.?The?quantitative?determination?was?conducted?by?ESI (+)?ionization?mode?and?multi-reaction?monitoring?(MRM).【Result】The?recovery?rates?of?trifloxystrobin?in coffee?fruits?ranged?from?87.8%?to?106.7%,?and?the?relative?standard?deviation?(RSD)?ranged?from?1.3%?to?5.8% when?the?additive?amount?of?trifloxystrobin?ranged?from?0.01?to?2.00?mg・kgC1 .?The?recovery?rates?of trifloxystrobin?in?coffee?beans?ranged?from?83.2%?to?88.1%,?and?the?RSD?ranged?from?2.0%?to?6.2%.?The recovery?rates?of?trifloxystrobn?acid?in?coffee?fruits?ranged?from?71.5%?to?106.0%,?and?the?RSD?ranged?from ? ? ? 收稿日期:2018C04C23 网络首发时间:2018C12C28?14:39:00 网络首发地址:http://kns.cnki.net/kcms/detail/44.1110.s.20181227.1104.034.html 作者简介:张蕊(1994―),女,硕士研究生,E-mail:[email protected];