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Article(id=1153433636956266552, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153433633999282214, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20241203004, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1733155200000, receivedDateStr=2024-12-03, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1752929608811, onlineDateStr=2025-07-19, pubDate=1742832000000, pubDateStr=2025-03-25, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1752929608811, onlineIssueDateStr=2025-07-19, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1752929608811, creator=13701087609, updateTime=1752929608811, updator=13701087609, issue=Issue{id=1153433633999282214, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='6', pageStart='1', pageEnd='322', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1752929608105, creator=13701087609, updateTime=1758086445549, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1175062977960096080, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153433633999282214, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1175062977960096081, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153433633999282214, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=114, endPage=121, ext={EN=ArticleExt(id=1153433637933539393, articleId=1153433636956266552, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Determination of 146 kinds of pesticide residues in animal derived food by enhanced matrix removal-lipid dispersion solid phase extraction purification coupled with gas chromatography-tandem mass spectrometry, columnId=1153429495274000613, journalTitle=Journal of Food Safety & Quality, columnName=Special Topic: Research and Detection of Pesticide and Veterinary Drug Residue, runingTitle=null, highlight=null, articleAbstract=

Objective To establish an analytical method for the determination of 146 kinds of pesticide residues in animal derived foods by enhanced matrix removal-lipid dispersion solid phase extraction (dSPE EMR-Lipid) and purification technology coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The 5 g sample were added to 2 mL ultrapure water, extracted with acetonitrile, freezed for 10 min, separated with QuEChERS EN-extraction package, cleaned-up with dSPE EMR-Lipid, then was detected by GC-MS/MS in dynamic multi-reaction monitoring (DMRM) mode. The analytes were quantified by matrix-matched standard curve method. Results The results showed that 146 kinds of pesticides had good linearities in the concentration of 5-320 μg/L, the linear correlation coefficient of the compounds were greater than 0.9939, and the limits of detection of the method were 0.04-10.91 μg/kg, the limits of quantification were 0.11-32.72 μg/kg. The average recoveries of 146 kinds of pesticides at the spiked level of 0.01, 0.02 and 0.10 mg/kg ranged from 61.3% to 119.3%, relative standard deviations were 0.15%-16.02%. Conclusion The method is simple in pre-treatment, convenient in operation, rapid, sensitive and accurate in detection, can meet the simultaneous detection requirements for multiple pesticide residues. It is suitable for preliminary screening and quantitative detection of multiple pesticide residues in animal derived food.

, correspAuthors=Hua-Li XUE, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, authorCompany=null, fund=null, authors=null, authorsList=Zhi-Min YANG, Hua-Li XUE, Xiu-Li PAN, Yun LI, Jian LI, Hui DING, Yun LI, Xiao-Hui XU, Ting CHEN), CN=ArticleExt(id=1153433663166473050, articleId=1153433636956266552, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=增强型脂质去除分散固相萃取净化-气相色谱-串联质谱法测定动物性食品中146种农药残留, columnId=1153429495479521513, journalTitle=食品安全质量检测学报, columnName=本期专题：农兽药残留研究与检测, runingTitle=null, highlight=null, articleAbstract=

目的 建立一种基于增强型脂质去除分散固相萃取(enhanced matrix removal-lipid dispersion solid phase extraction, dSPE EMR-Lipid)净化技术结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)测定动物性食品中146种农药残留量的分析方法。方法 在5 g样品中加入2 mL超纯水, 经乙腈提取, 冷冻10 min, QuEChERS-EN-盐包除水分离, 采用dSPE EMR-Lipid净化技术, GC-MS/MS动态多反应监测(dynamic multi-reaction monitoring, DMRM)模式监测, 基质匹配标准曲线法定量分析。结果 146种化合物在5~320 μg/L范围内线性关系良好, 相关系数均大于0.9939, 方法的检出限为0.04~10.91 μg/kg, 定量限为0.11~32.72 μg/kg。146种化合物在0.01、0.02和0.10 mg/kg 3个不同加标水平下的平均回收率范围在61.3%~119.3%之间, 相对标准偏差为0.15%~16.02%。结论 该方法操作简便快速, 灵敏准确, 能够满足多种农药残留量的同时检测需求, 适用于动物性食品中多种农药残留的定量筛查。

, correspAuthors=薛华丽, authorNote=null, correspAuthorsNote=
* 薛华丽(1977—), 女, 博士, 教授, 主要研究方向为采后生物学与技术和食品质量与安全。E-mail:
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杨志敏(1985—), 女, 硕士, 高级工程师, 主要研究方向为外源性污染物质的检测分析。E-mail:

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杨志敏(1985—), 女, 硕士, 高级工程师, 主要研究方向为外源性污染物质的检测分析。E-mail:

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杨志敏(1985—), 女, 硕士, 高级工程师, 主要研究方向为外源性污染物质的检测分析。E-mail:

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增强型脂质去除分散固相萃取净化-气相色谱-串联质谱法测定动物性食品中146种农药残留
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杨志敏 1 , 薛华丽 2, * , 潘秀丽 1 , 李运 1 , 李坚 1 , 丁辉 1 , 李赟 1 , 许晓辉 1 , 陈婷 1
食品安全质量检测学报 | 本期专题：农兽药残留研究与检测 2025,16(6): 114-121
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食品安全质量检测学报 | 本期专题：农兽药残留研究与检测 2025, 16(6): 114-121
增强型脂质去除分散固相萃取净化-气相色谱-串联质谱法测定动物性食品中146种农药残留
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杨志敏1 , 薛华丽2, * , 潘秀丽1, 李运1, 李坚1, 丁辉1, 李赟1, 许晓辉1, 陈婷1
作者信息
  • 1.兰州市食品药品检验检测研究院, 国家市场监督管理总局重点实验室/食品中农药兽药残留监控, 兰州 730050
  • 2.甘肃农业大学理学院, 兰州 730070

    • 杨志敏(1985—), 女, 硕士, 高级工程师, 主要研究方向为外源性污染物质的检测分析。E-mail:

通讯作者:

* 薛华丽(1977—), 女, 博士, 教授, 主要研究方向为采后生物学与技术和食品质量与安全。E-mail:
Determination of 146 kinds of pesticide residues in animal derived food by enhanced matrix removal-lipid dispersion solid phase extraction purification coupled with gas chromatography-tandem mass spectrometry
Zhi-Min YANG1 , Hua-Li XUE2, * , Xiu-Li PAN1, Yun LI1, Jian LI1, Hui DING1, Yun LI1, Xiao-Hui XU1, Ting CHEN1
Affiliations
  • 1. Lanzhou Institute for Food and Drug Control, Key Laboratory of Pesticide and Veterinary Drug Monitoring, State Administration for Market Regulation, Lanzhou 730050, China
  • 2. College of Science, Gansu Agricultural University, Lanzhou 730070, China
出版时间: 2025-03-25 doi: 10.19812/j.cnki.jfsq11-5956/ts.20241203004
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摘要
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目的 建立一种基于增强型脂质去除分散固相萃取(enhanced matrix removal-lipid dispersion solid phase extraction, dSPE EMR-Lipid)净化技术结合气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)测定动物性食品中146种农药残留量的分析方法。方法 在5 g样品中加入2 mL超纯水, 经乙腈提取, 冷冻10 min, QuEChERS-EN-盐包除水分离, 采用dSPE EMR-Lipid净化技术, GC-MS/MS动态多反应监测(dynamic multi-reaction monitoring, DMRM)模式监测, 基质匹配标准曲线法定量分析。结果 146种化合物在5~320 μg/L范围内线性关系良好, 相关系数均大于0.9939, 方法的检出限为0.04~10.91 μg/kg, 定量限为0.11~32.72 μg/kg。146种化合物在0.01、0.02和0.10 mg/kg 3个不同加标水平下的平均回收率范围在61.3%~119.3%之间, 相对标准偏差为0.15%~16.02%。结论 该方法操作简便快速, 灵敏准确, 能够满足多种农药残留量的同时检测需求, 适用于动物性食品中多种农药残留的定量筛查。

动物性食品  /  增强型脂质去除分散固相萃取  /  气相色谱-串联质谱法  /  农药残留

Objective To establish an analytical method for the determination of 146 kinds of pesticide residues in animal derived foods by enhanced matrix removal-lipid dispersion solid phase extraction (dSPE EMR-Lipid) and purification technology coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The 5 g sample were added to 2 mL ultrapure water, extracted with acetonitrile, freezed for 10 min, separated with QuEChERS EN-extraction package, cleaned-up with dSPE EMR-Lipid, then was detected by GC-MS/MS in dynamic multi-reaction monitoring (DMRM) mode. The analytes were quantified by matrix-matched standard curve method. Results The results showed that 146 kinds of pesticides had good linearities in the concentration of 5-320 μg/L, the linear correlation coefficient of the compounds were greater than 0.9939, and the limits of detection of the method were 0.04-10.91 μg/kg, the limits of quantification were 0.11-32.72 μg/kg. The average recoveries of 146 kinds of pesticides at the spiked level of 0.01, 0.02 and 0.10 mg/kg ranged from 61.3% to 119.3%, relative standard deviations were 0.15%-16.02%. Conclusion The method is simple in pre-treatment, convenient in operation, rapid, sensitive and accurate in detection, can meet the simultaneous detection requirements for multiple pesticide residues. It is suitable for preliminary screening and quantitative detection of multiple pesticide residues in animal derived food.

animal derived foods  /  enhanced matrix removal-lipid dispersion solid phase extraction  /  gas chromatography-tandem mass spectrometry  /  pesticide residues
杨志敏, 薛华丽, 潘秀丽, 李运, 李坚, 丁辉, 李赟, 许晓辉, 陈婷. 增强型脂质去除分散固相萃取净化-气相色谱-串联质谱法测定动物性食品中146种农药残留. 食品安全质量检测学报, 2025 , 16 (6) : 114 -121 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241203004
Zhi-Min YANG, Hua-Li XUE, Xiu-Li PAN, Yun LI, Jian LI, Hui DING, Yun LI, Xiao-Hui XU, Ting CHEN. Determination of 146 kinds of pesticide residues in animal derived food by enhanced matrix removal-lipid dispersion solid phase extraction purification coupled with gas chromatography-tandem mass spectrometry[J]. Journal of Food Safety & Quality, 2025 , 16 (6) : 114 -121 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241203004
正文
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0 引言
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化学农药在促进农产品增产的同时, 不仅影响生态环境, 还会通过环境、饲料、饮水、呼吸、食物链等多种途径引入到动物性食品中, 造成农药在动物性食品中的残留[1-2]。随着人们对动物性食品需求的增加, 残留的农药通过食物链可能在人体内蓄积, 对人体健康造成潜在危害[3-4]。
农药残留是全球重点关注的一项指标, 许多国家制定了严格的动物性食品的农药最大残留限量(maximum residue limit, MRL)。随着对农药种类覆盖范围的增加, 对限量值的严格要求, 这对检测方法的简便、快速、灵敏及通量的需求提出了更高的要求。目前涉及动物性食品检验方法的标准和文献报道主要有气相色谱法(gas chromatograph, GC)[5-6]、气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)[7-10]、气相色谱-串联质谱法(gas chromatography- tandem mass spectrometry, GC-MS/MS)[11-12]、液相色谱-串联质谱法(liquid chromatography- tandem mass spectrometry, LC-MS/ MS)[13-17]、高分辨质谱法[18-19]等。GC-MS和LC-MS/MS是国家标准和文献报道中最常用的方法, 关于GC-MS/MS检测方法的国家标准相对较少。采用GC-MS/MS高通量检测多种农药残留, 多数报道的是针对植物性食品, 对检测动物性食品中多种农药残留的高通量方法相对较少, 因此, 对动物性食品建立准确、灵敏的高通量检测方法是非常必要的。
动物性食品中含有大量的脂肪和蛋白质, 不仅会污染仪器, 还可能干扰目标农药的检测, 去除脂肪是动物性样品前处理的关键。目前关于动物性食品中的农药多残留分析所报道的前处理方法中多数采用凝胶渗透色谱[20-22]、固相萃取法[23-24]、冷冻过滤技术[25]、QuEChERS前处理[26-27]等, 且多数是与LC-MS/MS结合进行检测。凝胶渗透色谱设备昂贵, 操作烦琐, 不利于批量检测; 固相萃取前处理操作复杂、耗时长; QuEChERS具有成本低、快速便捷、萃取效率高等特点, 近年来虽被广泛应用, 但是在多农残检测中存在净化材料选择局限性等缺点。增强型脂质去除分散固相萃取(enhanced matrix removal-lipid dispersion solid phase extraction, dSPE EMR-Lipid)作为一种新型吸附材料, 能够选择性去除样品提取物中的主要脂类, 不会造成分析物的损失, 在兽药残留检测中去脂效果较好[28], 鉴于此, 本研究以乙腈为提取溶剂, dSPE EMR-Lipid净化, 浓缩、置换溶剂复溶后以GC-MS/MS定量分析, 建立一种简便、快速、准确测定动物性食品中农药多残留的分析方法, 为动物性食品的质量安全提供技术保障。
1 材料与方法
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1.1 试剂、仪器与材料
146种农药标准品(纯度≥95%, 天津阿尔塔科技有限公司); N-丙基乙酰胺(N-primary secondary amine, PSA)、碳十八烷基硅烷键合硅胶(C18)、QuEChERS-EN-提取包(内含氯化钠1 g、无水MgSO4 4 g、柠檬酸钠1 g、柠檬酸氢二钠0.5 g)、dSPE EMR-Lipid净化管(美国Agilent科技有限公司); 羟基多壁碳纳米管(hydroxylated multi-walled carbon nanotubes, MWCNTs-OH)、多壁碳纳米管(multi-walled carbon nanotubes, MWCNTs)(中国科学院成都有机化学有限公司); ZIP-8(兰州化物所合成); 无水硫酸镁(分析纯, 国药集团化学试剂有限公司); 乙酸乙酯、乙腈(色谱纯, 德国Merck公司); 丙酮(色谱纯, 科密欧化学试剂有限公司)。
7890B-7000D气相色谱-三重四极杆质谱联用仪、HP-5 MS UI毛细管色谱柱(30 m×0.25 mm, 0.25 μm)(美国Agilent科技有限公司); Milli-Q超纯水机(美国Millipore公司); AUTO-EVA-60全自动平行浓缩仪(睿科集团股份有限公司); 5810R高速低温离心机(德国Eppendor公司); VORTEX-5涡旋混匀器(海门其林贝尔公司); T 18匀浆机(德国IKA公司); JR05-300绞肉机(浙江苏泊尔股份有限公司)。
猪肉、牛肉、羊肉、鸡肉、水产品、鸡蛋样品均为市售。
1.2 样品制备
猪肉、牛肉、羊肉、鸡肉: 将肉去筋膜, 切成小块, 绞肉机充分绞碎成糜状; 水产品: 按照GB/T 30891—2014《水产品抽样规范》, 取可食部分用匀浆机制备; 蛋类: 去壳后用搅拌机搅匀, 制成匀浆。
1.3 样品前处理
称取5 g(精确至0.001 g)匀浆样品至50 mL离心管中, 加入2 mL超纯水, 充分摇匀, 准确加入10 mL乙腈, 超声提取10 min, 置于-18 ℃冷冻10 min, 然后加入QuEChERS-EN-提取盐包, 快速摇散, 涡旋混合1 min, 4000 r/min离心5 min (4 ℃条件下), 收集上清液。准确移取3.0 mL上清液于预先装有净化材料的dSPE EMR-Lipid净化管中, 涡旋混合1 min, 以4000 r/min离心5 min (4 ℃条件下), 取净化液2.0 mL至10 mL离心管中, 于40 ℃水浴中氮吹至近干, 准确加入1.0 mL乙酸乙酯复溶, 过0.22 μm有机滤膜, 收集滤液, 上机测试。
1.4 标准溶液的配制
标准储备溶液配制: 分别精确称取10 mg单个农药标准品于10 mL容量瓶中, 用丙酮定容至刻度; 混合标准工作溶液配制: 精密移取单个储备溶液, 用乙酸乙酯定容, 配制成1000 μg/L的标准工作溶液。临用时用乙酸乙酯或者空白基质样品溶液(按1.3方法制备)将混合标准工作液配制成系列标准溶液, 所有标准溶液均置于棕色瓶内于-18 ℃密封保存, 备用。
1.5 仪器条件
1.5.1 色谱条件
色谱柱: HP-5 MS UI毛细管色谱柱(30 m×0.25 mm, 0.25 μm); 程序升温: 初始温度60 ℃(保持1 min), 以40 ℃/min升温至170 ℃, 再以10 ℃/min升温至310 ℃(保持3 min); 进样口温度: 280 ℃; 流速: 1.0 mL/min; 进样模式: 不分流进样; 进样量: 1 μL。
1.5.2 质谱条件
离子源: 电子轰击(electron impact, EI)源; 电离能量: 70 eV; 离子源温度: 230 ℃; 辅助传输线温度: 280 ℃; 溶剂延迟2.5 min; 监测模式: 动态多反应监测模式; 碰撞气: 氮气; 淬灭气: 氦气(纯度均≥99.999%)。图1为猪肉基质中146种农药的总离子流图。
1.6 数据处理
采用Agilent MassHunter软件对农药化合物定性和定量分析, 采用Excel 2019软件对数据进行统计分析、制表及绘图。
2 结果与分析
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2.1 加水量的选择
前处理技术是分析痕量组分过程中极为重要的环节, 主要是提取、净化、浓缩和复溶等步骤。我国2018年以后发布的多个农药残留检测标准和文献[12]报道多数以乙腈为提取溶剂。肉类样品具有一定的黏性, 脂肪在乙腈中的溶解度较小, 蛋白质在乙腈作用下会变性沉淀, 这会使目标物被包裹难以释放[29], 加水后可将样品分散均匀, 增强乙腈对样品的渗透性, 有利于目标物提取[30], 同时考虑到后期还需加盐除去多余水分, 本研究考察5 g样品分别加入0、2、5 mL超纯水, 经前处理后对目标化合物回收率的影响(见图2)。结果显示, 未净化时, 回收率在60%~120%范围内化合物数量从高到低为2 mL>0 mL>5 mL, 加水量2 mL时, 回收率低于60%或高于120%的数量最少。净化后, 不同加水量的平均回收率均高于未净化, 加水量2 mL时, 目标化合物整体平均回收率最高, 不加水时, 回收率高于120%的化合物偏多, 加水量5 mL时, 回收率低于60%的化合物数量增加。因此, 本研究以5 g样品中加入2 mL超纯水为宜。
2.2 净化条件的选择
动物性食品的基质成分复杂, 萃取液中的杂质不仅会影响目标化合物的离子化效率和响应强度, 导致灵敏度下降, 还会造成仪器堵塞, 降低色谱柱寿命。通过对提取液有效净化, 可降低检测干扰和仪器污染。目前常用的净化材料有C18、PSA、碳基纳米材料(MWCNTs、MWCNTs-OH), 以及去脂材料dSPE EMR-Lipid等。本研究考察C18、PSA、MWCNTs、MWCNTs-OH、dSPE EMR-Lipid以及实验室自备合成的ZIP-8净化材料等实验方案(如方案: ① MgSO4 450 mg+PSA 30 mg、② MgSO4 450 mg+C18 30 mg、③ MgSO4 450 mg+PSA 15 mg+C18 15 mg、④ MgSO4 450 mg+MWCNTs 30 mg、⑤ MgSO4 450 mg+ MWCNTs-OH 30 mg、⑥ dSPE EMR-Lipid、⑦ ZIP-8 30 mg)对农药化合物净化效果的影响(图3)。图3结果显示, 比较回收率在60%~120%的农药数量, 方案③和⑥较其他方案均好, 且在此范围内方案⑥的平均回收率(91.3%)较方案③的平均回收率(89.3%)高。同时考虑到要实际应用于大批量样本的快速处理, 最终选择dSPE EMR-Lipid净化填料为本研究的净化方案。
2.3 基质效应
基质效应(matrix effect, ME)是基质匹配标准曲线斜率与溶剂标准曲线斜率之差与溶剂标准曲线斜率的百分比。当ME为正时, 表现为基质增强效应; 负时则为基质抑制效应。当|ME|低于20%时, ME可忽略不计; |ME|高于50%时, 表现为强ME; |ME|介于20%~50%之间, 则为中等ME[18](图4)。考察了146种农药在空白猪肉中的ME结果表明, 92.5%的农药表现为基质增强效应, 7.5%的农药表现为基质抑制效应。其中24.7%的农药ME可忽略, 37.0%的农药为中等ME, 38.3%的农药为强ME。考虑到定量的准确度, 则需绘制基质匹配标准曲线来降低ME的影响。
2.4 方法学考察
采用系列基质混合标准工作液(5~320 μg/L)定量分析, 以农药质量浓度(X, μg/L)为横坐标, 农药浓度响应的峰面积(Y)为纵坐标, 绘制标准曲线, 通过线性拟合得到回归方程和相关系数。按照GB 5009.295—2023《食品安全国家标准 化学分析方法验证通则》采用空白猪肉基质样品加标稀释测定, 分别以信噪比为3和10时表示方法的估算检出限(limit of detection, LOD)和估算定量限(limit of quantification, LOQ)。加标回收率实验设置3水平(0.01、0.02、0.10 mg/kg), 每个水平平行测定6次考察该方法的准确度和精密度。146种农药的相关系数、LODs、LOQs、回收率和精密度结果见表1。结果表明, 146种农药的线性关系良好, 相关系数均不低于0.9939, 化合物的LODs为0.04~10.91 μg/kg, LOQs为0.11~32.72 μg/kg, 146种化合物在3个水平下的回收率范围为61.3%~119.3%, 其中3个水平下回收率在70%~120%的化合物分别占91.1%、97.3%和96.6%。相对标准偏差(relative standard deviation, RSD)为0.15%~16.02%, 结果表明该方法的LOD和LOQ可以满足日常监测需求; 虽然有少数化合物的回收率不是很理想, 但该方法可以满足动物源性食品中多数农药化合物的定量筛查。
2.5 实际样品测定
采用本研究建立的方法对猪肉、牛肉、羊肉、鸡肉、鱼肉和鸡蛋各10批样品进行检测。结果显示, 1批鸡肉中检出啶酰菌胺(1.80 μg/kg), 2批鸡蛋中检测出氟虫腈砜(1.74 μg/kg、1.90 μg/kg), 5批鱼肉中均检出4,4,-滴滴伊(1.80~2.18 μg/kg), 其含量均远低于GB 2763—2021《食品安全国家标准 食品中农药最大残留限量》的限量要求, 色谱图详见图5。此外, 5批鱼肉中有其他农药检出, 包括氟铃脲、二甲戊灵, 噻呋酰胺、氰戊菊酯, 测定含量均高于LOQ, 但其在GB 2763—2021中均未规定限量要求, 按照日本《食品中残留农业化学品肯定列表制度》[31]规定的“一律标准”限量值为10 μg/kg, 有3批鱼肉中的氟铃脲高于此限量要求, 其他样品均未检出农药残留。可见, 鱼肉中农药残留的风险值得关注。
3 结论
收起
本研究以dSPE EMR-Lipid净化技术为前处理的去脂手段, 结合GC-MS/MS建立一种快速、准确测定动物性食品中146种农药残留的定性定量分析方法。该前处理方法操作简便, 净化效果好, 可有效降低基质中的杂质干扰, 选择性和准确度高, 适用于动物性食品中多种农药残留的同时测定分析, 可为动物性食品中多农药残留的日常监测和监管提供技术支撑, 也可为后续标准的制修订提供参考。
基金
收起
  • 甘肃省市场监督管理局科技计划项目(SSCJG-SP-A202308)
  • 兰州市青年科技人才创新项目(2023-QN-180)
  • 兰州市科技发展指导性计划项目(2023-ZD-234)
  • 兰州市科技发展指导性计划项目(2024-9-227)
  • 兰州市科技计划项目(2023-3-29)
文献
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doi: 10.19812/j.cnki.jfsq11-5956/ts.20241203004
  • 接收时间：2024-12-03
  • 首发时间：2025-07-19
  • 出版时间：2025-03-25
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  • 收稿日期：2024-12-03
基金
甘肃省市场监督管理局科技计划项目(SSCJG-SP-A202308)
兰州市青年科技人才创新项目(2023-QN-180)
兰州市科技发展指导性计划项目(2023-ZD-234)
兰州市科技发展指导性计划项目(2024-9-227)
兰州市科技计划项目(2023-3-29)
作者信息
    1.兰州市食品药品检验检测研究院, 国家市场监督管理总局重点实验室/食品中农药兽药残留监控, 兰州 730050
    2.甘肃农业大学理学院, 兰州 730070

通讯作者:

* 薛华丽(1977—), 女, 博士, 教授, 主要研究方向为采后生物学与技术和食品质量与安全。E-mail:
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https://castjournals.cast.org.cn/joweb/spaq/CN/10.19812/j.cnki.jfsq11-5956/ts.20241203004
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2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
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