Department of Chemistry, College of Basic Science and Humanities, Govind Ballabh Pant University of Agriculture and Technology, Pantnagar, Uttarakhand, 263145, India.
Anal Sci. 2023 Apr;39(4):431-439. doi: 10.1007/s44211-022-00227-y. Epub 2022 Dec 1.
Pesticides are widely employed to boost the production of vegetable crops, but their indiscriminate application leaves residue in the crops for long, even after harvesting. Among pesticides, neonicotinoids are the most commonly applied group of insecticides which are used on vegetables to defend against a variety of sucking pests. The purpose of this study was to validate an analytical approach focused on QuEChERS extraction for the validation and simultaneous determination of residues of four neonicotinoids (imidacloprid, clothianidin, acetamiprid and thiamethoxam) in six diverse crops such as cucumber, brinjal, tomato, beans, cabbage, and cauliflower. Insecticides were quantified using high-performance liquid chromatography (HPLC) fitted with a UV-Vis detector. Specificity, linearity, precision, accuracy, limit of detection, and the limit of quantification were all considered for validation. The fortification of the vegetables was done at three different levels (0.2, 0.3 and 0.5 µg mL), for confirming the validity of the method adopted. The results demonstrated adequate recoveries ranging from 77.5 to 96.4% and good accuracy (RSDs between 0.3 and 8.9%). For all the insecticides, the approach had good linearity with R ≥ 0.99. The limit of detection (LOD) and the limit quantification (LOQ) levels of all the four analytes were 0.05 µg mL and 0.2 µg mL, respectively. The validation characteristics of the devised method are satisfactory in terms of specificity, linearity, precision, accuracy, limit of detection and limit of quantification and thus can be successfully employed for simultaneous determination of the neonicotinoids.
农药被广泛用于提高蔬菜作物的产量，但它们的滥用量会导致残留物在作物中长时间存在，即使在收获后也是如此。在农药中，烟碱类杀虫剂是最常用的杀虫剂之一，用于蔬菜防治各种吸汁害虫。本研究旨在验证一种基于 QuEChERS 提取的分析方法，用于验证和同时测定六种不同作物（黄瓜、茄子、番茄、豆类、白菜和花椰菜）中四种新烟碱类杀虫剂（吡虫啉、噻虫嗪、噻虫胺和噻虫啉）的残留量。使用配备紫外可见检测器的高效液相色谱法（HPLC）定量杀虫剂。对特异性、线性、精密度、准确度、检测限和定量限进行了验证。通过在三个不同水平（0.2、0.3 和 0.5 µg mL）对蔬菜进行添加，以确认所采用方法的有效性。结果表明，回收率在 77.5%至 96.4%之间，准确度良好（RSD 在 0.3%至 8.9%之间）。对于所有杀虫剂，该方法均具有良好的线性关系，R 值≥0.99。所有四种分析物的检测限（LOD）和定量限（LOQ）水平分别为 0.05 µg mL 和 0.2 µg mL。该方法在特异性、线性、精密度、准确度、检测限和定量限方面的验证特性令人满意，因此可成功用于同时测定新烟碱类杀虫剂。
