Chowdhury Nushrat Jahan, Akbor Md Ahedul, Nahar Aynun, Ali Shaikh Md Aftab
Institute of National Analytical Research and Services (INARS), Bangladesh Council of Scientific and Industrial Research (BCSIR), Dhaka, Bangladesh.
Department of Chemistry, University of Dhaka, Dhaka, Bangladesh.
Heliyon. 2024 Jul 14;10(14):e34548. doi: 10.1016/j.heliyon.2024.e34548. eCollection 2024 Jul 30.
Organochlorine pesticides (OCPs) are persistent organic compounds found in aquatic environments worldwide. A well-validated and well-established analytical method is crucial for detecting OCPs in the environment. In this study, an analytical method for quantifying OCPs in water was developed and evaluated. Here, the range of linearity, reproducibility, uncertainty, specificity, method detection limits (MDL), and special emphasis on detection and quantitation limits were assessed. Recovery studies were performed to measure the accuracy and precision of the method. This method exhibited excellent linearity in the range of 2.5-20 μg/L for all compounds. As none of the targeted compounds was detected in the chromatograms of the blank sample with no baseline noise, the limits of detection (LOD) and limits of quantification (LOQ) were determined using the linear regression method, external calibration curve slope, and laboratory fortified blank-based detection. All compounds showed different LOD and LOQ values, depending on the approach used. In particular, endosulfan sulfate, methoxychlor, endrin ketone, H. epoxide, heptachlor, and 4,4'-DDT exhibited high detection limits. The recovery percentage of the 15 compounds at 5 μg/L spiked concentration was between 50 and 150 %, which is consistent with the accuracy of the APHA method. Except for endosulfan sulfate, the relative standard deviations of all other compounds were below 20 %, indicating good precision. This method has also been applied to real water samples. This validation technique is reliable, sensitive, simple, rapid, easy to comprehend, and reproducible. The application of this method in the real water samples was also conducted. Only α-BHC and γ-Chlordane were detected in the water sample.
有机氯农药（OCPs）是在全球水生环境中发现的持久性有机化合物。一种经过充分验证且成熟的分析方法对于检测环境中的OCPs至关重要。在本研究中，开发并评估了一种定量水中OCPs的分析方法。在此，评估了线性范围、重现性、不确定度、特异性、方法检测限（MDL），并特别强调了检测限和定量限。进行了回收率研究以测量该方法的准确性和精密度。该方法对所有化合物在2.5 - 20μg/L范围内均表现出良好的线性。由于在无基线噪声的空白样品色谱图中未检测到任何目标化合物，因此使用线性回归法、外标校准曲线斜率和基于实验室加标空白的检测来确定检测限（LOD）和定量限（LOQ）。所有化合物根据所采用的方法显示出不同的LOD和LOQ值。特别是，硫丹硫酸酯、甲氧滴滴涕、异狄氏剂酮、环氧七氯、七氯和4,4'-滴滴涕表现出较高的检测限。15种化合物在5μg/L加标浓度下的回收率在50%至150%之间，这与美国公共卫生协会（APHA）方法的准确性一致。除硫丹硫酸酯外，所有其他化合物的相对标准偏差均低于20%，表明精密度良好。该方法也已应用于实际水样。这种验证技术可靠、灵敏、简单、快速、易于理解且可重现。还进行了该方法在实际水样中的应用。在水样中仅检测到α-六六六和γ-氯丹。
