Biswas A K, Rao G S, Kondaiah N, Anjaneyulu A S R, Malik J K
Division of Livestock Products Technology, Indian Veterinary Research Institute, Izatnagar 243122 (UP), India.
J Agric Food Chem. 2007 Oct 31;55(22):8845-50. doi: 10.1021/jf071140w. Epub 2007 Oct 4.
A simple, specific, and rapid analytical method for the determination of trimethoprim (TMP) and three sulfonamide (SA) antimicrobial drug residues in buffalo meat is developed and validated. This method is based on a solid-phase extraction technique followed by high-performance liquid chromatography (HPLC)-photodiode array (PDA) detection. Target compounds were extracted from the meat by acetonitrile and water, cleaned up on a Bond Elute C 18 cartridge column, and separated on a RP-C 18 column during HPLC analysis. Acetonitrile along with water appears to be an excellent extractant as recovery of the analytes at maximum residues levels (MRLs) in spiked sample was in the range of 75-108%, with coefficient of variations (CVs) ranging between 1.34 and 22%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.031 and 0.062 microg/g, respectively, for all of the compounds. Intra- and interday assay precisions of the method at 0.125 microg/g concentrations for any drug ranged between 3 and 4%. The linearities of the TMP, sulfadimidine (SDM), sulfadoxine (SDO), and sulfamethoxazole (SMX) were 0.9989, 0.9999, 0.9998, and 0.9997, respectively. For robustness, the analytical method was applied to 122 buffalo meat samples obtained from export meat processing plants.
建立并验证了一种简单、特异且快速的分析方法,用于测定水牛肉中甲氧苄啶(TMP)和三种磺胺类(SA)抗菌药物残留。该方法基于固相萃取技术,随后进行高效液相色谱(HPLC)-光电二极管阵列(PDA)检测。目标化合物通过乙腈和水从肉中提取,在Bond Elute C 18柱上净化,并在HPLC分析期间在RP-C 18柱上分离。乙腈和水似乎是一种出色的萃取剂,加标样品中最大残留限量(MRLs)下分析物的回收率在75-108%范围内,变异系数(CVs)在1.34%至22%之间。所有化合物的检测限(LOD)和定量限(LOQ)分别为0.031和0.062微克/克。该方法在0.125微克/克浓度下对任何药物的日内和日间测定精密度在3%至4%之间。TMP、磺胺二甲嘧啶(SDM)、磺胺多辛(SDO)和磺胺甲恶唑(SMX)的线性分别为0.9989、0.9999、0.9998和0.9997。为评估稳健性,将该分析方法应用于从出口肉类加工厂获得的122份水牛肉样品。