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固相萃取-高效液相色谱-二极管阵列检测法测定生咖啡中七种新烟碱类农药的含量

SPE-HPLC-DAD Dosage of Seven Neonicotinoids in Green Coffee.

作者信息

Seccia Serenella, Albrizio Stefania, Dini Irene

机构信息

Department of Pharmacy, University of Naples Federico II, Via Domenico Montesano 49, 80131 Napoli, Italy.

出版信息

Molecules. 2025 Apr 26;30(9):1930. doi: 10.3390/molecules30091930.

Abstract

Green coffee is essential in many tropical economies. Its cultivation often necessitates using pesticides that can leave behind residues harmful to human health. To ensure consumer safety, the European Community has set strict maximum residue limits (ranging from 0.01 to 1.0 mg/kg) for pesticides in green coffee sold within Europe. However, the lack of official testing methods for neonicotinoids (NEOs) is a problem, as laboratories must spend resources and time developing and validating suitable analytical methods. This study developed and validated a method for the simultaneous analysis of seven NEOs frequently used in coffee cultivation: acetamiprid, clothianidin, dinotefuran, imidacloprid, nitenpyram, thiacloprid, and thiamethoxam. The proposed methodology uses Strata-X PRO cartridges (solid-phase extraction) to remove interfering compounds present in the food matrix and high-performance liquid chromatography (HPLC), equipped with a diode array detector (DAD), to determine NEOs. The accuracy profile strategy validated the method's suitability for the intended application. NEO recovery rates above 97%; negligible matrix effects (>93%); the linearity of the quantification method (R values above 0.99); relative biases and standard deviations below 5% and 6%, respectively; and an expected error rate less than 8% allowed to consider the method reliable for the intended objectives. Because of its low ecological impact and simple execution, this method can be used in routine analyses.

摘要

生咖啡豆在许多热带经济体中至关重要。其种植往往需要使用农药,而这些农药可能会残留对人体健康有害的物质。为确保消费者安全,欧洲共同体对在欧洲销售的生咖啡豆中的农药设定了严格的最大残留限量(范围为0.01至1.0毫克/千克)。然而,缺乏针对新烟碱类农药(NEOs)的官方检测方法是个问题,因为实验室必须花费资源和时间来开发和验证合适的分析方法。本研究开发并验证了一种同时分析咖啡种植中常用的七种新烟碱类农药的方法:啶虫脒、噻虫胺、呋虫胺、吡虫啉、烯啶虫胺、噻虫啉和噻虫嗪。所提出的方法使用Strata-X PRO柱(固相萃取)去除食品基质中存在的干扰化合物,并使用配备二极管阵列检测器(DAD)的高效液相色谱(HPLC)来测定新烟碱类农药。准确性概况策略验证了该方法适用于预期应用。新烟碱类农药的回收率高于97%;基质效应可忽略不计(>93%);定量方法的线性(R值高于0.99);相对偏差和标准偏差分别低于5%和6%;预期误差率小于8%,这些都使得该方法被认为对于预期目标是可靠的。由于其对生态的影响较小且执行简单,该方法可用于常规分析。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/04ed/12073578/9b256168bc97/molecules-30-01930-g001.jpg

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