关键词: Insecticide Micellar liquid chromatography Residue Washing

Mesh : Cicer / chemistry Spinacia oleracea / chemistry Insecticides / analysis isolation & purification Plant Leaves / chemistry Micelles Pesticide Residues / analysis isolation & purification Chromatography, Liquid / methods Limit of Detection Reproducibility of Results

来  源:   DOI:10.1016/j.chroma.2024.465043

Abstract:
In the past few decades, the employment of green analytical approaches in chromatographic method development has attracted the analytical separation community. The greenness of the developed method depends upon the toxicity of solvents and the amount of generated post-analysis waste generated. In this concern, micellar liquid chromatography (MLC) is a simple and rapid technique that generates very low toxic waste compared to traditional chromatographic pesticide detection methods. Here, MLC method has been validated and applied for the determination of monocrotofos (MCF), imidacloprid (ICP), dimethoate (DM) and profenofos (PFF) in spinach and chickpea leaves. The optimized mobile phase was 0.065 M SDS-2 % 1-propanol, 0.01 M NaH2PO4 buffered to pH 7. A C18 column was used for separation with a flow rate of 1 mL/min. The developed method has been validated following the guidelines of SANTE/11,312/2021 and ICH guidelines for; limit of quantification (0.05-0.20 mg/kg), linearity (r2> 0.997-0.999), precision (<6.3 %), accuracy (96.3 %-99.8 %) and robustness (<6) in real samples. ICP and MCF, apart from DM and PFF, were detected in the present work. After detecting insecticides in spinach and chickpea leaves both were washed with different household chemicals i.e. normal, lukewarm, common salt, lemon juice water and commercial ozonizer. Based on five washing techniques with insecticide concentration time intervals reduction rates were calculated for each washing treatment. The results show that lemon juice, common salt water, and ozonizer can be used as washing techniques for the reduction of superficial and systematic residues of ICP and MCF. Common salt and lemon juice water were better for washing over vinegar and potassium permanganate (KMnO4) as they enhance the colour of the green leafy vegetables and are available in every Indian kitchen. They can be easily used by lower socioeconomic classes who cannot afford KMnO4 and vinegar.
摘要:
在过去的几十年里,绿色分析方法在色谱方法开发中的应用吸引了分析分离界。所开发方法的绿色度取决于溶剂的毒性和所产生的分析后废物的产生量。在这个问题上,胶束液相色谱(MLC)是一种简单快速的技术,与传统的色谱农药检测方法相比,其产生的毒性非常低。这里,MLC方法已经过验证,并用于单色磷(MCF)的测定,吡虫啉(ICP),菠菜和鹰嘴豆叶中的乐果(DM)和丙苯糖(PFF)。优化的流动相为0.065MSDS-2%1-丙醇,0.01MNaH2PO4缓冲至pH7。使用C18柱进行分离,流速为1mL/min。所开发的方法已根据SANTE/11,312/2021和ICH指南进行了验证;定量限(0.05-0.20mg/kg),线性度(r2>0.997-0.999),精度(<6.3%),真实样本的准确性(96.3%-99.8%)和稳健性(<6)。ICP和MCF,除了DM和PFF,在目前的工作中被发现。在菠菜和鹰嘴豆叶中检测到杀虫剂后,都用不同的家用化学品洗涤,即正常的,不温不火,食盐,柠檬汁水和商用臭氧发生器。基于具有杀虫剂浓度时间间隔的五种洗涤技术,计算了每种洗涤处理的减少率。结果表明,柠檬汁,普通盐水,和臭氧发生器可用作洗涤技术,以减少ICP和MCF的表面和系统残留物。食盐和柠檬汁水更适合用醋和高锰酸钾(KMnO4)洗涤,因为它们可以增强绿叶蔬菜的颜色,并且可以在每个印度厨房中使用。它们可以很容易地被那些负担不起KMnO4和醋的较低社会经济阶层使用。
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