Yoshikawa Souichi, Nagano Chieko, Kanda Maki, Hayashi Hiroshi, Matsushima Yoko, Nakajima Takayuki, Tsuruoka Yumi, Nagata Marie, Koike Hiroshi, Sekimura Kotaro, Hashimoto Tsuneo, Takano Ichiro, Shindo Tetsuya
Tokyo Metropolitan Institute of Public Health, Shinju-ku, Tokyo 169-0073, Japan.
Tokyo Metropolitan Institute of Public Health, Shinju-ku, Tokyo 169-0073, Japan.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Jul 1;1057:15-23. doi: 10.1016/j.jchromb.2017.04.041. Epub 2017 Apr 26.
We developed a simultaneous determination method for 37 veterinary drugs in two chicken processed foods (deep-fried chicken and non-fried chicken cutlet) and muscle via liquid chromatography-mass spectrometry. The veterinary drugs belong to 7 different classes, including 4 antifolics, 4 benzimidazoles, 5 macrolides, 7 polyethers, 2 quinolones, 7 sulfonamides, and 8 other classes. The samples were extracted with ethyl acetate followed by acetonitrile with salt and buffers extraction. The two-step extraction enabled analyte extraction from highly lipid samples. The clean-up procedure, a solid-supported liquid extraction clean-up using a diatomaceous earth mini-cartridge, eliminated lipid co-extraction. The prepared sample matrix did not have an effect on the 36 analytes. The method was validated in accordance with the requirements of Japanese validation guidelines. Almost all targeted veterinary drugs successfully satisfied the guideline criteria in the three types of food matrices. The method exhibited recoveries of 70-105%, and the precision of repeatability and within-laboratory reproducibility ranged from 1 to 11% and 1 to 15%, respectively. The limits of quantification were estimated to range from 0.2 to 1.0μg/kg. Applying this method to samples commercially available in Tokyo, residues were detected in 3 out of 26 deep-fried chickens, 5 out of 20 non-fried chicken cutlets, and 17 out of 39 chicken muscles.
我们开发了一种通过液相色谱-质谱联用同时测定两种鸡肉加工食品(炸鸡和无骨炸鸡排)及肌肉中37种兽药的方法。这些兽药分属7个不同类别,包括4种抗叶酸剂、4种苯并咪唑类、5种大环内酯类、7种聚醚类、2种喹诺酮类、7种磺胺类以及8种其他类别。样品先用乙酸乙酯萃取,再用含盐和缓冲液的乙腈萃取。两步萃取法能够从高脂样品中萃取出分析物。净化步骤采用硅藻土微型柱进行固相萃取净化,可消除脂质的共萃取。制备好的样品基质对36种分析物没有影响。该方法按照日本验证指南的要求进行了验证。在这三种食品基质中,几乎所有目标兽药均成功满足指南标准。该方法的回收率为70%-105%,重复性精密度和实验室内再现性精密度分别为1%-11%和1%-15%。定量限估计为0.2-1.0μg/kg。将该方法应用于东京市售的样品,在26份炸鸡中有3份、20份无骨炸鸡排中有5份以及39份鸡肉中有17份检测到了兽药残留。