液质联用检测水产品中氯霉素、氟苯尼考和甲砜氯霉素的残留量

Determination of Chloramphenicol, Florfenicol and Thiamphenicol Residues in Aquatic Product by Lipid Chromatography-mass/mass Spectrometry

建立了采用液相色谱一质谱同位素稀释法同时测定水产品中氯霉素、氟苯尼考、甲砜氯霉素三种残留药物的方法。样品采用碱化乙酸乙酯提取，同位素内标法定量。氯霉素、氟苯尼考、甲砜氯霉素三种药物的定量限（LOQ）分别为0．05ng/mL、0．5ng/mL、0．7ng/mL；药物质量浓度分别在0．05-1．2ng/g、0．5-20．0ng/g和0．7-28．0ng/g内，与相应的峰面积比值呈良好的线性关系，并且在鱼肉中氯霉素、氟苯尼考、甲砜氯霉素回收率分别为92．2％-125．5％、78．6％-102．7％和79．4％-121．0％，在虾肉中分别为98．5％-128．4％、73．5％-109．6％和87．7％-122．8％。该法具有简单、快速、简化样品前处理步骤等优点。

A method for identification and qualification of Chloramphenicol, Florfenicol and Thiamphenicol residues in aquatic product was developed with the internal standard method and micro preprocessing method, which could avoid the solid phase extraction steps. The limit of quantization （LOQ） of Chloramphenicol, Florfenicol and Thiamphenicol residues were 0.05 ng/mL, 0.5 ng/mL and 0.7 ng/mL, respectively, with a recovery ranged from 80 to 120 %. And the corresponding concentration of the three compounds were within range of 0.05-1.2 ng/g, 0.5-20.0 ng/g and 0.7-28.0 ng/g, respectively, showing a good linear relationship between peak area ratios and correlation coefficient. The method were simple, fast and efficient, which can meet the needs of determination and quantization of related compounds in aquatic foodstuffs.