Manzano-Sánchez Lorena, Angappan Suganthi, Martínez José Antonio, Del Real Aguilera Ana, Fernández-Alba Amadeo Rodríguez
European Union Reference Laboratory for Pesticide Residues in Fruits & Vegetables, Agrifood Campus of International Excellence (ceiA3), University of Almeria, Ctra. Sacramento S/N˚, La Cañada de San Urbano, 04120, Almeria, Spain.
Tamil Nadu Agricultural University, Coimbatore, 641003, Tamil Nadu, India.
Anal Bioanal Chem. 2023 Nov;415(26):6551-6560. doi: 10.1007/s00216-023-04933-y. Epub 2023 Sep 12.
Spices such as paprika, curry, turmeric, dry chilli, and black pepper are grown in various geographic locations and widely used by consumers across the world. Pesticides applied during crop production practices could contaminate the produce, affecting the quality and posing a health risk for consumers. The complexity of the spice matrix and the wide range of target pesticides potentially present require special sample extraction and clean-up treatments to overcome matrix interference and ion suppression. In this study, sample extracts from spice matrices (paprika/curry/turmeric/dry chilli/black pepper) were cleaned up by an automated µSPE clean-up method for multi-residue analysis of pesticides using LC-MS/MS. The automated µSPE clean-up method involves pre-filled cartridges containing various sorbent materials suitable for numerous co-extractives and the automated clean-up process was carried out using an autosampler. The regulatory limit for pesticides in spices varies with type, with a low MRL of 0.05 mg kg or higher for 99% of the analytes. At spiking concentrations of 0.05 and 0.1 mg kg, good recoveries between 70 and 120% with RSD values below 20% were achieved for more than 98% of the compounds. With automatic clean-up of samples that takes 5 min/sample, 20% increased output per day shows an important advantage achieved compared to manual clean-up.
辣椒粉、咖喱、姜黄、干辣椒和黑胡椒等香料在不同地理位置种植，被世界各地的消费者广泛使用。作物生产过程中使用的农药可能会污染农产品，影响其质量，并对消费者构成健康风险。香料基质的复杂性以及可能存在的多种目标农药，需要特殊的样品提取和净化处理，以克服基质干扰和离子抑制。在本研究中，通过一种自动化的微固相萃取（µSPE）净化方法对香料基质（辣椒粉/咖喱/姜黄/干辣椒/黑胡椒）的样品提取物进行净化，用于使用液相色谱-串联质谱（LC-MS/MS）对农药进行多残留分析。自动化的µSPE净化方法涉及预装含有各种吸附材料的小柱，这些吸附材料适用于多种共萃取物，并且使用自动进样器进行自动化净化过程。香料中农药的监管限量因类型而异，99%的分析物最低残留限量（MRL）为0.05 mg/kg或更高。在0.05和0.1 mg/kg的加标浓度下，超过98%的化合物回收率在70%至120%之间，相对标准偏差（RSD）值低于20%。样品自动净化每个样品只需5分钟，与手动净化相比，每天产量提高20%显示出了一个重要优势。
