Zhang Dan, Park Jin-A, Kim Seong-Kwan, Cho Sang-Hyun, Cho Soo-Min, Shim Jae-Han, Kim Jin-Suk, Abd El-Aty A M, Shin Ho-Chul
Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul, Republic of Korea.
Biotechnology Research Institute, College of Agriculture and Life Sciences, Chonnam National University, Gwangju, Republic of Korea.
Biomed Chromatogr. 2017 Jun;31(6). doi: 10.1002/bmc.3891. Epub 2016 Dec 14.
In this study, an analytical method was developed for quantification of residues of the anthelmintic drug phenothiazine (PTZ) in pork muscle using liquid chromatography-tandem mass spectrometry. Muscles were extracted using 0.2% formic acid and 10 mm ammonium formate in acetonitrile, defatted and purified using n-hexane. The drug was well separated on a Waters XBridge™ C analytical column using a binary solvent system consisting of 0.2% formic acid and 10 mm ammonium formate in ultrapure water (A) and acetonitrile (B). Good linearity was achieved over a six-point concentration range in matrix-matched calibration with determination coefficient =0.9846. Fortified pork muscle having concentrations equivalent to and double the limit of quantification (1 ng/g) yielded recovery ranges between 100.82 and 104.03% and relative standard deviations <12%. Samples (n = 5) collected from large markets located in Seoul City tested negative for PTZ residue. In conclusion, 0.2% formic acid and ammonium formate in acetonitrile can effectively extract PTZ from pork muscle without solid-phase extraction, a step normally required for cleanup before analysis and the validated method can be used for routine analysis to ensure the quality of animal products.
在本研究中,开发了一种使用液相色谱 - 串联质谱法测定猪肌肉中驱虫药吩噻嗪(PTZ)残留量的分析方法。肌肉用乙腈中的0.2%甲酸和10 mM甲酸铵进行提取,用正己烷脱脂和纯化。该药物在Waters XBridge™ C分析柱上使用由超纯水中的0.2%甲酸和10 mM甲酸铵(A)以及乙腈(B)组成的二元溶剂系统得到了良好的分离。在基质匹配校准的六点浓度范围内实现了良好的线性,测定系数 = 0.9846。添加浓度相当于定量限(1 ng/g)及其两倍的猪肌肉的回收率范围为100.82%至104.03%,相对标准偏差<12%。从首尔市大型市场采集的样本(n = 5)PTZ残留检测呈阴性。总之,乙腈中的0.2%甲酸和甲酸铵无需固相萃取即可有效地从猪肌肉中提取PTZ,固相萃取通常是分析前净化所需的步骤,且该验证方法可用于常规分析以确保动物产品质量。