液质联用法同时测定牛和山羊组织中的三氯苯达唑及其代谢物。
Simultaneous determination of triclabendazole and its metabolites in bovine and goat tissues by liquid chromatography-tandem mass spectrometry.
机构信息
Key Laboratory of Veterinary Drug Safety Evaluation and Residues Research, Shanghai Veterinary Research Institute, Chinese Academy of Agricultural Sciences, 518 Ziyue Road, Minhang, 200241 Shanghai, People's Republic of China.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Nov 15;878(30):3106-12. doi: 10.1016/j.jchromb.2010.09.018. Epub 2010 Sep 29.
A sensitive liquid chromatography-tandem mass spectrometry method for the simultaneous determination of triclabendazole, its main metabolites (triclabendazole sulphone and triclabendazole sulphoxide) and a marker residue (ketotriclabendazole) in bovine and goat muscle, liver, and kidney samples is developed and validated. Analyte extraction from samples is effectively performed using liquid-liquid extraction by acetonitrile. Chromatographic separation is performed on a C₁₈ reversed-phase column with gradient elution. The analytes are detected by tandem quadrupole mass spectrometry after positive electrospray ionization by multiple reaction monitoring. The limits of detection for analytes are found to be 0.25-2.5 μg/kg in muscle tissues and 1-10 μg/kg in liver and kidney tissues, respectively. The recoveries of edible bovine and goat tissues range from 84.9% to 109.5% when spiked at different levels with analytes, with relative standard deviations generally below 12.8%.
建立并验证了一种同时测定牛和山羊肌肉、肝脏和肾脏组织中三氯苯达唑、其主要代谢物（三氯苯达唑砜和三氯苯达唑亚砜）和一个残留标志物（酮三氯苯达唑）的灵敏液相色谱-串联质谱检测方法。采用乙腈液-液萃取法，从样品中有效提取分析物。采用 C₁₈反相柱进行色谱分离，梯度洗脱。通过正电喷雾电离，多反应监测进行串联四极杆质谱检测。在肌肉组织中的检测限为 0.25-2.5μg/kg，在肝脏和肾脏组织中的检测限为 1-10μg/kg。当在不同水平下用分析物对可食用的牛和山羊组织进行加标时，回收率在 84.9%至 109.5%之间，相对标准偏差通常低于 12.8%。
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