Pesticide Toxicology Laboratory, Department of Agricultural Entomology, Tamil Nadu Agricultural University, Coimbatore 641 003, Tamil Nadu, India.
Bull Environ Contam Toxicol. 2012 Nov;89(5):1051-6. doi: 10.1007/s00128-012-0789-2. Epub 2012 Aug 22.
A multiresidue method was developed and optimized for the quantification of organochlorine pesticides (OCPs) in milk, egg and meat samples. Sample extraction was performed by adopting QuEChERS principle and the extracts were cleaned-up dispersive solid-phase extraction with primary secondary amine after salting out with NaCl and MgSO(4). Analysis was carried out by gas chromatography coupled with electron capture detector and confirmation by gas chromatography-mass spectrometry. The performance of the method was investigated in terms of linearity, accuracy, precision, detection limit and quantification limit (LOQ). Good linearity was obtained, with correlation coefficients (r(2)) higher than 0.992. Mean recoveries were found in the ranges 72%-108%, 74%-101% and 75.27%-104.56% for the milk, egg and meat, respectively, RSD % turned out to range from 0.28% to 10.05%. The method developed was successfully tested on commercial milk, egg, and meat samples from the markets of Tamil Nadu (India), proving to be a useful tool in routine analysis of OCPs for monitoring purposes. None of the compounds of interest were observed above their respective LOQ.
建立并优化了一种用于牛奶、鸡蛋和肉类样品中有机氯农药(OCPs)定量分析的多残留方法。采用 QuEChERS 原理提取样品,在盐析后用 NaCl 和 MgSO4 提取,用初级/次级胺进行分散固相萃取净化。采用气相色谱-电子捕获检测器进行分析,并用气相色谱-质谱法进行确证。该方法的性能通过线性、准确度、精密度、检测限和定量限(LOQ)进行了研究。结果表明,方法具有良好的线性,相关系数(r2)均高于 0.992。牛奶、鸡蛋和肉类中的平均回收率分别在 72%-108%、74%-101%和 75.27%-104.56%范围内,RSD%在 0.28%-10.05%之间。该方法已成功应用于印度泰米尔纳德邦市场的商业牛奶、鸡蛋和肉类样品的检测,可作为监测 OCPs 的常规分析的有用工具。在所研究的化合物中,均未观察到高于各自 LOQ 的含量。