Department of Chemistry, College of Science, United Arab Emirates University, P.O. Box 15551, Al-Ain, Abu Dhabi, United Arab Emirates.
Department of Statics, College of Business and Economics, United Arab Emirates University, P.O. Box 15551, Al-Ain, Abu Dhabi, United Arab Emirates.
J Dairy Sci. 2024 Apr;107(4):1916-1927. doi: 10.3168/jds.2023-23512. Epub 2023 Nov 2.
This study aimed to use ultra-high-performance liquid chromatography coupled to a triple-quadrupole mass spectrometer to detect 11 carbamate pesticide residues in raw and pasteurized camel milk samples collected from the United Arab Emirates. A method was developed and validated by evaluating limits of detection, limits of quantitation, linearity, extraction recovery, repeatability, intermediate precision, and matrix effect. Due to the high protein and fat content in camel milk, a sample preparation step was necessary to avoid potential interference during analysis. For this purpose, 5 different liquid-liquid extraction techniques were evaluated to determine their efficiency in extracting carbamate pesticides from camel milk. The established method demonstrated high accuracy and precision. The matrix effect for all carbamate pesticides was observed to fall within the soft range, indicating its negligible effect. Remarkably, detection limits for all carbamates were as low as 0.01 μg/kg. Additionally, the coefficients of determination were >0.998, demonstrating excellent linearity. A total of 17 camel milk samples were analyzed, and only one sample was found to be free from any carbamate residues. The remaining 16 samples contained at least one carbamate residue, yet all detected concentrations were below the recommended maximum residue limits set by Codex Alimentarius and the European Union pesticide databases. Nonetheless, it is worth noting that the detected levels of ethiofencarb in 3 samples were close to the borderline of the maximum residue limit. To assess the health risk for consumers of camel milk, the hazard index values of carbofuran, carbaryl, and propoxur were calculated. The hazard index values for these 3 carbamate pesticides were all below 1, indicating that camel milk consumers are not at risk from these residues.
本研究旨在使用超高效液相色谱-串联三重四极杆质谱法检测从阿拉伯联合酋长国采集的生骆驼奶和巴氏杀菌骆驼奶样品中的 11 种氨基甲酸酯类农药残留。通过评估检测限、定量限、线性、提取回收率、重复性、中间精密度和基质效应，开发并验证了一种方法。由于骆驼奶中蛋白质和脂肪含量较高，因此需要进行样品前处理步骤，以避免分析过程中潜在的干扰。为此，评估了 5 种不同的液液萃取技术，以确定它们从骆驼奶中提取氨基甲酸酯农药的效率。所建立的方法表现出较高的准确性和精密度。所有氨基甲酸酯农药的基质效应均观察到处于软范围，表明其影响可忽略不计。值得注意的是，所有氨基甲酸酯的检测限均低至 0.01μg/kg。此外，相关系数均>0.998，表现出极好的线性。共分析了 17 份骆驼奶样品，只有一份样品未检出任何氨基甲酸酯残留。其余 16 个样品均至少含有一种氨基甲酸酯残留，但所有检测到的浓度均低于食品法典委员会和欧盟农药数据库规定的最大残留限量。然而，值得注意的是，在 3 个样品中检测到的乙硫苯威接近最大残留限量的边界。为评估消费者食用骆驼奶的健康风险，计算了克百威、涕灭威和丙硫克百威的危害指数值。这 3 种氨基甲酸酯农药的危害指数值均低于 1，表明骆驼奶消费者不存在这些残留的风险。
