MAO Key Laboratory of Food Safety Evaluation/National Reference Laboratory of Veterinary Drug Residues (HZAU), Huazhong Agricultural University, Wuhan, Hubei, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Jun 1;879(19):1659-67. doi: 10.1016/j.jchromb.2011.04.004. Epub 2011 Apr 12.
A confirmatory and quantitative method of liquid chromatography-tandem mass spectrometry (LC-MS/MS) combined with a pressure liquid extraction (PLE) was developed for the determination of 11 benzimidazole and 10 metabolites of albendazole, fenbendazole and mebendazole in the muscles and livers of swine, cattle, sheep and chicken. For sample preparation, we used an automated technique of PLE method. The optimum extraction conditions were obtained using an 11 ml Accelerated Solvent Extraction (ASE) cells, acetonitrile/hexane as the extraction solvent. HPLC analysis was performed on a C18 column with gradient elution using acetonitrile and 5 mmol l(-1) formic ammonium as mobile phase. The analytes were detected in the positive ion multiple reaction monitoring (MRM) mode by the LC-ESI-MS/MS analysis. The recoveries of benzimidazole (BZDs) spiked at the levels of 0.5 μg kg(-1) ranged from 70.1% to 92.7%; the between-day relative standard deviations were no more than 10%. The limits of quantification were 0.02-0.5 μg kg(-1). The optimized method was successfully applied to monitor real samples containing BZDs, demonstrating the method to be simple, fast, robust and suitable for identification and quantification of BZDs residues in animal products.
建立了一种液质联用（LC-MS/MS）结合加压液体萃取（PLE）的确证定量方法，用于检测猪肉、牛肉、羊肉和鸡肉肌肉和肝脏中 11 种苯并咪唑类药物和阿苯达唑、芬苯达唑和甲苯达唑的 10 种代谢物。对于样品制备，我们使用了 PLE 方法的自动化技术。通过使用 11ml 的加速溶剂萃取（ASE）细胞、乙腈/正己烷作为萃取溶剂，获得了最佳的萃取条件。HPLC 分析在 C18 柱上进行，采用乙腈和 5mmol l（-1）甲酸铵作为流动相进行梯度洗脱。通过 LC-ESI-MS/MS 分析，以正离子多反应监测（MRM）模式检测分析物。苯并咪唑（BZDs）在 0.5μgkg（-1）水平的添加回收率在 70.1%至 92.7%之间；日间相对标准偏差不超过 10%。定量限为 0.02-0.5μgkg（-1）。优化后的方法成功应用于监测含有 BZDs 的实际样品，证明该方法简单、快速、稳健，适用于动物产品中 BZDs 残留的鉴定和定量。
