Pagliuca Giampiero, Gazzotti Teresa, Zironi Elisa, Sticca Patrizia
Department of Veterinary Public Health and Animal Pathology, Food Hygiene and Technology Section, Alma Mater Studiorum, University of Bologna, Via Tolara di Sopra, 50 I 40064 Ozzano Emilia, BO, Italy.
J Chromatogr A. 2005 Apr 15;1071(1-2):67-70. doi: 10.1016/j.chroma.2004.08.142.
Organophosphorus pesticides (OPPs) were determined in matrices of animal origin by dual column capillary gas chromatography using nitrogen-phosphorus detection (NPD). This method was tested on cow milk and on liver and muscle of wild boar. The isolation of these pesticides was performed by liquid partition followed by cleanup with solid phase cartridge (SPE C18), after extraction from the matrix. The analytes identification was obtained by comparing the retention times in two columns with different polarity. The quantification of each OPP was obtained using parathion-ethyl as internal standard. The method was developed in a UNI EN ISO 9001:2000 certified laboratory. The recovery, investigated by analyzing samples spiked at 5, 10 and 50 ppb, ranged from 59 to 117% in milk, from 60 to 81% in liver and from 68 to 76% in muscle. The limit of quantification (LOQ) and limit of detection (LOD) were, respectively, 5 and 1 ppb for each compound and allowed quantifying the residues below the legal limits.
采用双柱毛细管气相色谱法并结合氮磷检测（NPD）测定动物源基质中的有机磷农药（OPPs）。该方法在牛奶以及野猪的肝脏和肌肉上进行了测试。这些农药的分离是在从基质中提取后，通过液液分配，然后用固相萃取柱（SPE C18）净化来完成的。通过比较在两根不同极性的色谱柱上的保留时间来进行分析物的鉴定。使用对硫磷乙酯作为内标对每种OPPs进行定量。该方法是在一个通过UNI EN ISO 9001:2000认证的实验室中开发的。通过分析添加浓度为5、10和50 ppb的加标样品进行回收率研究，牛奶中的回收率在59%至117%之间，肝脏中的回收率在60%至81%之间，肌肉中的回收率在68%至76%之间。每种化合物的定量限（LOQ）和检测限（LOD）分别为5 ppb和1 ppb，能够对低于法定限量的残留进行定量。
