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荔枝中20种登记农药残留分析方法研究

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为解决荔枝中20种登记农药多残留的同时快速检测问题,建立并优化基于超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测荔枝中7种杀虫剂和13种杀菌剂的分析方法.荔枝全果样品经80%乙腈水溶液提取后,用石墨化碳黑(GCB)净化,流动相为乙腈和水,梯度洗脱,采用Extend C18色谱柱进行分离.电喷雾正负离子交替模式采集,多反应监测(MRM),外标法定量.20种供试农药的质量浓度与其对应的峰面积之间呈现良好线性关系,相关系数均大于0.9990;20种农药在荔枝基质中的平均回收率为71%～106%,相对标准偏差(RSD)在0.9%～9.8%之间,满足残留分析的要求.该方法简便、高效,可用于荔枝样品中20种农药残留的快速检测.
Determination of Residues of Twenty Registered Pesticides in Lychee
The paper aims to solve the problem of simultaneous and rapid detection of 20 registered pesticide residues in lychee.An analytical method based on ultra-high performance liquid chromatography-tandem mass spectrometry was established and optimized for simultaneous determination of 7 insecticides and 13 fungicides in lychee.The whole lychee fruit were extracted with 80%acetonitrile aqueous solution and cleaned up with graphitized carbon black(GCB).Extend C18 chromatographic column was used for separation and the mobile phase was acetonitrile and water by gradient elution.Electrospray ionization in positive and negative ion mode was selected,the detection mode was multi-reaction monitoring,and external standard method was used for quantification.The results showed that a good linear relationship was presented between the mass concentration and peak area of the twenty tested pesticides,and the determination coefficient was greater than 0.9990.The average recoveries of the twenty pesticides in lychee were in range of 71%-106%with the relative standard deviations(RSD)of 0.9%-9.8%,which met the requirements of residue analysis.The results demonstrated that the proposed method was convenient and effective for the quick determination of these twenty pesticides residues in lychee.

ultra-high performance liquid chromatography-tandem mass spectrometrylycheeinsecticidefungicideresidue

王思威、刘艳萍、张树飞、张惠云、何强、王潇楠、常虹

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广东省农业科学院植物保护研究所/农业农村部华南果蔬绿色防控重点实验室/广东省植物保护新技术重点实验室,广州 510640

深圳职业技术大学食品药品学院,深圳 518000

云南省农业科学院热带亚热带经济作物研究所,云南保山 678000

广东省农产品质量安全中心,广州 525000

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超高效液相色谱-串联质谱 荔枝 杀虫剂 杀菌剂 残留

现代农业产业技术体系建设项目乡村振兴战略专项农业科技能力提升项目乡村振兴战略专项农业科技能力提升项目广州市科技计划广州市科技计划广东省基础和应用基础研究基金

CARS-322023TS-2-52023TS-2-32022010104792023A04J08052022A1515110473

2024

中国农学通报
中国农学会

中国农学通报

CSTPCD
影响因子：0.891
ISSN：1000-6850
年,卷(期)：2024.40(13)