气相色谱-串联质谱法和液相色谱-串联质谱法快速测定葡萄中45种农药残留-食品安全质量检测学报-CSCIED科技核心评价数据库-手机版

气相色谱-串联质谱法和液相色谱-串联质谱法快速测定葡萄中45种农药残留

Rapid determination of 45 kinds of pesticide residues in Vitis vinifera by gas chromatography-tandem mass spectrometry and liquid chromatography-tandem mass spectrometry

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DOI	10.19812/j.cnki.jfsq11-5956/ts.20241218006
刊名	食品安全质量检测学报 Journal of Food Safety and Quality
年，卷(期)	2025, 16(12)
作者	史晓梅, 张巍巍, 武进普, 吕朝政, 高曼, 蔡沅锟, 钱承敬, 丁子元*,
作者单位	中粮营养健康研究院; 北京市营养健康与食品安全重点实验室
摘要	目的建立气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)和液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)快速检测葡萄中45种农药残留的分析方法。方法葡萄样品使用乙腈经振荡提取和超声辅助提取后, 上清液用混合吸附填料进行分散固相萃取净化, 高速离心后过滤膜, 分别用GC-MS/MS的选择反应监测(selected reaction monitoring, SRM)模式和LC-MS/MS的多反应监测(multiple reaction monitoring, MRM)模式进行检测。结果溴氰菊酯在0.1~1.0 mg/kg、克菌丹在0.2~3.0 mg/kg、甲霜灵等28种农药在0.04~1.00 mg/kg、甲氨基阿维菌素苯甲酸盐等15种农药在0.1~1.0 mg/kg的浓度范围内具有良好的线性关系, 相关系数达到0.99以上。检出限为0.00020~0.05000 mg/kg, 定量限为0.00050~0.15000 mg/kg。45种农药在3个不同加标水平的平均加标回收率为70.3%~117.0%, 相对标准偏差为0.01%~14.30%。结论本方法无需复杂样品前处理设备即可实现葡萄中45种农药残留的快速检测, 准确性好, 操作简便, 能够很好满足葡萄中多农药残留日常监测分析工作的要求。
Abstract	Objective To establish a method for the rapid determination of 45 kinds of pesticides residues in Vitis vinifera by gas chromatography-tandem mass spectrometry (GC-MS/MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods The Vitis vinifera samples were first extracted with acetonitrile by vibration and ultra-sonic. Then the mix adsorbents were used in dispersive solid phase extraction to purify the extract. After high speed centrifugation and filtration, the samples were detected by GC-MS/MS using selected reaction monitoring (SRM) mode, and LC-MS/MS using multiple reaction monitoring (MRM) mode. Results Deltamethrin exhibited good linearity within the concentration range of 0.1 to 1.0 mg/kg, while captan showed linearity within the range of 0.2 to 3.0 mg/kg, 28 kinds of pesticides including metalaxyl showed good linear relationships within the concentration range of 0.04–1.00 mg/kg, and 15 kinds of pesticides including emamectin benzoate showed good linear relationships within the concentration range of 0.1–1.0 mg/kg, with correlation coefficients reached 0.99 or above. The limits of detection were in the range of 0.00020–0.05000 mg/kg, the limits of quantitation were in the range of 0.00050–0.15000 mg/kg. The spiked recoveries at 3 levels of 45 kinds of pesticides were in range of 70.3%–117.0%, the relative standard deviations were in range of 0.01%–14.30%. Conclusion With features such as accuracy and easy operation, this method can be used to fast determination of 45 kinds of pesticides in Vitis vinifera without any special samples pretreatment apparatus, and also satisfies the requirement of pesticide routine analysis.
关键词	多农药残留；QuEChERS；气相色谱-串联质谱法；液相色谱-串联质谱法；葡萄；快速测定
KeyWord	multiple pesticide residues; QuEChERS; gas chromatography-tandem mass spectrometry; liquid chromatography-tandem mass spectrometry; Vitis vinifera; rapid determination
基金项目
页码	77-87

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引用本文

史晓梅, 张巍巍, 武进普, 吕朝政, 高曼, 蔡沅锟, 钱承敬, 丁子元*. 气相色谱-串联质谱法和液相色谱-串联质谱法快速测定葡萄中45种农药残留 [J]. 食品安全质量检测学报. 2025; 16; (12). 77 - 87.

文献评论

柳**安徽理工****** 已认证✔

2025-11-28 10:46:07

该论文聚焦葡萄中45种农药残留快速检测方法，建立了QuEChERS结合GC-MS/MS与LC-MS/MS的分析方法，符合我国食品安全监管实际，具有一定的应用价值。研究设计较为科学合理，优化了提取溶剂与净化填料用量，明确了两种质谱技术的检测参数，覆盖45种常用农药，线性范围适配实际残留水平，相关系数均达0.99以上，精准性较好。方法学验证较为全面，检出限低至0.00020 mg/kg，定量限≤0.15000 mg/kg，加标回收率70.3%~117.0%，相对标准偏差≤14.30%，满足痕量分析的准确性与精确性的要求。创新点在于将超声辅助提取与QuEChERS净化结合，无需复杂前处理设备，操作简便、成本低廉，适配实验室日常监测。实际样品检测验证了方法实用性，为葡萄质量安全管控提供了技术支撑。不足在于未深入探讨基质效应影响，对不同品种葡萄的适用性有待一步验证。总体而言，论文实验设计严谨，数据可靠，结论明确，是一篇兼具科学性与应用价值的研究论文，可用于葡萄农药残留常规检测。

陈**郑州大学****** 已认证✔

2025-11-06 02:09:45

本文针对葡萄中多农药残留检测的复杂性与多样性问题，建立了基于 QuEChERS前处理结合GC-MS/MS与LC-MS/MS双平台检测的高通量分析方法，具有明显的实用性与创新性。研究思路清晰，实验设计合理，充分体现了“快速、准确、简便”的技术特点。在方法学层面，作者通过优化提取溶剂、分散固相萃取吸附剂比例及仪器参数，实现了对45种不同理化性质农药的同时测定，回收率范围广而稳定（70.3%–117.0%），RSD低于15%，数据充分证明了方法的可靠性与适用性。值得肯定的是，研究中系统考察了色素干扰与基质效应的抑制策略，使检测结果更具代表性和准确度。该研究成果为葡萄及其他果蔬中多农药残留的常规监测与风险评估提供了重要技术参考，具有较高的推广价值与行业指导意义。总体而言，论文结构完整、数据翔实、结论可信，是一篇兼具学术性与应用性的高质量研究论文。

刘**新疆维吾****** 已认证✔

2025-10-14 05:44:32

论文建立了一种基于QuEChERS-GC-MS/MS与LC-MS/MS联用技术的葡萄中45种农药残留快速检测方法，具有重要的现实意义和应用价值。研究亮点在于通过系统优化，特别是创新性地确定了GCB用量，有效解决了色素干扰与平面农药回收率低的关键难题；方法学验证数据详实，线性、回收率及RSD等指标均符合残留分析要求，且在实际样品中成功检出多种农药残留，证明了其可靠性。总体而言，该方法简便、准确、灵敏，完全满足葡萄中多农残快速筛查的需求，是一篇质量较高的应用研究论文。

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