水产品中氯霉素、甲砜霉素、氟苯尼考、氟苯尼考胺多残留的同时测定—GC/MS法

Simultaneous Determination of Chloramphenicol, Thiamphenicol, Florfenicol and Florfenicol Amine Residues in Aquatic Products with Gas Chromatography/Mass Spectrometry

中文关键词: 气相色谱-质谱法  氯霉素  甲砜霉素  氟苯尼考  氟苯尼考胺  水产品  多残留

英文关键词: Gas chromatography/mass spectrometry (GC/MS)  Chloramphenicol  Thiamphenicol  Florfenicol  Florfenicol amine  Aquatic products  Multi-residue

中文摘要:

      采用气相色谱质谱法建立基质加标标准曲线，对中国对虾、大菱鲆、鲫鱼、鳗鱼、蟹、甲鱼6种主要养殖水产品肌肉组织中氯霉素类药物：氯霉素(CAP)、甲砜霉素(TAP)、氟苯尼考(FF)及其代谢物氟苯尼考胺(FFA)的多残留同时进行检测。结果显示，CAP在2–200 ng/ml浓度范围内，线性关系良好；TAP、FF和FFA在5–200 ng/ml浓度范围内，线性关系良好，其相关系数均大于0.990。加标回收率在76.4%–94.3%之间，相对标准偏差在5.7%–13.9%之间。检出限：CAP为0.2 μg/kg，TAP、FF和FFA均为1.0 μg/kg。定量限：CAP为0.5 μg/kg，TAP、FF和FFA均为3.0 μg/kg。研究表明，该方法具有准确、高效、灵敏、特异性强的特点，可以满足水产品中CAP、TAP、FF和FFA多残留的同时检测的要求。

英文摘要:

      In this study we used major aquatic products in china (Penaeus chinensis, turbot, carp, river eels, crabs and turtles) as the experimental materials to explore the simultaneous detection of multiple residues of chloramphenicol drugs [Chloramphenicol (CAP), Thiamphenicol (TAP), Florfenicol (FF) and its metabolites-Florfenicol amine (FFA)] in the muscle tissues of aquatic products, and the method of Gas chromatography-Mass spectrometry was established. Samples were extracted with ethyl acetate and ammonium hydroxide (v : v = 98 : 2), degreased with n-hexane, and further defatted with the Oasis MCX solid phase extraction cartridge. Then the samples were derivatized with the silanization reagent and negative chemical ionization (NCI). The selected ion monitoring mode (SIM) was applied in the experiments. The selected ions of the four drugs were as below: CAP m/z 376, 378, 466*, 468; TAP m/z 409*, 411, 499, 411; FF m/z 339*, 341, 429, 341; FFA m/z 209*, 194, 210, 194 (*quantitative ion). The matrix spiked calibration curve was established. There was a clear linear relationship in the ranges of 2−200 ng/ml for CAP and 5−200 ng/ml for TAP, FF and FFA, and the correlation coefficients were more than 0.990. The recovery was 75%−110%, and the relative standard deviation was 5.7%−13.9%. The detection limit was 0.2 μg/kg for CAP, and 1.0 μg/kg for TAP, FF and FFA. These results indicated that the GC/MS method could be accurate, efficient, sensitive and highly specific. Therefore it may satisfy the simultaneous determination of the four target compounds in aquatic products.