UPLC-MS/MS法检测黄鳝中氯霉素类药物残留  

Determination of chloramphenicols in the eels by UPLC-MS / MS

作　　者：彭麟[1] 郭大伟[1] 张伟[1] 阮祥春[1] 高修歌[1] 高颖[1] 李娇娇[1] 郑亚妮[1] 季辉[1] 江善祥[1] 

机构地区：[1]南京农业大学动物医学院,江苏南京210095

出　　处：《畜牧与兽医》2016年第4期30-35,共6页Animal Husbandry & Veterinary Medicine

摘　　要：建立一种检测黄鳝肌肉中氯霉素、甲砜霉素和氟苯尼考残留的超高效液相色谱-串联质谱(UPLC-MS/MS)方法。黄鳝肌肉样品中加入无水硫酸钠和氯化钠,20 m L碱性乙酸乙酯提取2次。合并提取液,于45℃水浴中氮吹至干。5%甲醇溶液复溶,再加正己烷(5%甲醇溶液饱和)除脂。弃去上层正己烷,下层水相过0.22μm滤膜,进样检测。氯霉素、甲砜霉素和氟苯尼考在0.5~50μg·L^(-1)添加水平内线性良好,检测限为0.1μg·kg^(-1),定量限为0.3μg·kg^(-1)。氯霉素在0.3、0.45和0.6μg·kg^(-1)添加水平回收率为92.83%~111.26%;甲砜霉素在25、50和75μg·kg^(-1)添加水平回收率为86.76%~107.30%;氟苯尼考在50、100和150μg·kg^(-1)添加水平回收率为96.21%~104.14%。本方法对3种药物的平均提取回收率在86.76%~111.26%范围内,日内精密度为2.16%~13.66%,日间精密度为1.42%~8.06%。本研究建立的方法精密度高,重现性好,在保证回收率的基础上有效地提高了检测效率。The aim of this experiment was to establish an ultra performance liquid chromatography-tandem mass spectrometry（ UPLC-MS /MS） method to detect chloramphenicol,thiamphenicol and florfenicol residues in the eel muscles. Twenty millilitres of alkaline ethyl acetate was used to extract chloramphenicols in the tissue under adding anhydrous sodium sulfate and sodium chloride. The combined elution was evaporated to dryness under nitrogen stream in a water bath maintained at 45 ℃. The residues were reconstituted in 5% methanol solution together with n-hexane saturated by 5% methanol to remove fat. The upper layer of n-hexane was discarded,and the lower aqueous phase was poured through a 0. 22 μm filter into UPLC-MS / MS. The results showed that the calibration curves were good linear at the concentrations of0. 5 - 50 μg·L（-1）. The detection limit of chloramphenicol,thiamphenicol and florfenicol was 0. 1 μg·kg-（-1）and the limit of quantification was 0. 3 μg· kg-（-1）. The average recoveries of chloramphenicol at concentrations of 0. 3,0. 45 and 0. 6 μg · kg-（-1）were from 92. 83% to111. 26%,thiamphenicol at 25,50 and 75 μg·kg-（-1）ranged from 86. 76% to 107. 30% and florfenicol at 50,100 and 150 μg·kg-（-1）were from 96. 21% to 104. 14%. The average recoveries were from 86. 76% to 111. 26%,the Intra-day RSD of this method was from 2. 16% to13. 66%,and the Inter-day RSD was from 1. 42% to 8. 06%. In conclusion,the method established in this study greatly improved detection efficiency on the basis of ensuring the recovery.

关 键 词：UPLC-MS/MS 氯霉素 甲砜霉素 氟苯尼考 黄鳝 

分 类 号：S859.7[农业科学—临床兽医学]