Analytical Sciences Group, ASSIST Division, CSIR-Indian Institute of Toxicology Research, (CSIR-IITR), Vishvigyan Bhawan, 31, Mahatma Gandhi Marg, Lucknow, 226001, Uttar Pradesh, India; Academy of Scientific and Innovative Research (AcSIR), Ghaziabad, 201002, India.
Analytical Sciences Group, ASSIST Division, CSIR-Indian Institute of Toxicology Research, (CSIR-IITR), Vishvigyan Bhawan, 31, Mahatma Gandhi Marg, Lucknow, 226001, Uttar Pradesh, India.
Talanta. 2025 Jan 1;282:126968. doi: 10.1016/j.talanta.2024.126968. Epub 2024 Sep 27.
The widespread use of pesticides and their consequential presence in the environment is a growing concern due to the harmful health effects associated with pesticide exposure. For clinical and toxicology laboratories, a method for simultaneously determining these compounds and their metabolic products in body fluids, such as blood and urine, is important. In the present study, a rapid, sensitive and simultaneous LC-QToF-MS method for detecting multiclass pesticides and metabolites in blood and urine samples has been developed and validated. Four sample preparation procedures, protein precipitation and three different variants of QuEChERS-based extraction were evaluated to find a suitable, simple, and effective sample pretreatment technique. The final optimized sample preparation method (acetonitrile; 400 μl, MgSO; 40 mg and NaCl; 10 mg) was validated for accuracy, precision, matrix effect, recovery, stability, carryover, and dilution integrity. Analyte recoveries ranged from 75.40 to 113.54 % while accuracy was evaluated in the range of 71.41-108.26 % and precision (%RSD) in the range of 0.01 %-16.85 %. The limit of quantification (LOQ) for all compounds was established in the range of 0.82-7.05 ng mL. The developed reliable, robust, and sensitive method was successfully applied for the quantification of target pesticides and metabolites in human blood and urine samples. Evaluated samples resulted in detection of eleven analytes (seven pesticides and four metabolites).
由于与农药接触相关的有害健康影响,农药的广泛使用及其在环境中的存在是一个日益令人关注的问题。对于临床和毒理学实验室而言,重要的是开发和验证一种能够同时测定这些化合物及其代谢产物在血液和尿液等体液中的方法。在本研究中,建立并验证了一种快速、灵敏、同时测定血液和尿液样品中多类农药及其代谢物的 LC-QToF-MS 方法。评估了四种样品制备程序(蛋白质沉淀和三种不同的 QuEChERS 衍生提取方法),以找到合适、简单、有效的样品预处理技术。最终优化的样品制备方法(乙腈;400μl、MgSO4;40mg 和 NaCl;10mg)经过准确性、精密度、基质效应、回收率、稳定性、交叉污染和稀释完整性验证。分析物的回收率在 75.40%至 113.54%之间,而准确度在 71.41%至 108.26%之间,精密度(%RSD)在 0.01%至 16.85%之间。所有化合物的定量限(LOQ)均在 0.82-7.05ngmL 范围内。所开发的可靠、稳健、灵敏的方法成功应用于人体血液和尿液样品中目标农药及其代谢物的定量检测。评估的样本检测到了十一种分析物(七种农药和四种代谢物)。