气相色谱法同时测定水产品中氯霉素、氟甲砜霉素和甲砜霉素残留量

Simultaneous Determination of Residues of Chloramphenicol,Florfenicol,and Thiamphenicol in Fishery Products by Gas Chromatography

以尼罗罗非鱼（Oreochromis niloticus）和南美白对虾（Penaeus vannamei）为实验材料，建立了测定水产品中氯霉素、氟甲砜霉素和甲砜霉素残留量的毛细管电子捕获气相色谱（GC-ECD）法。用乙酸乙酯同时提取水产品中的待测物，提取液浓缩至干后溶于甲醇／氯化钠溶液，正己烷脱脂，过C18柱净化，乙腈洗脱，加BSTFA-TMCS在65℃下衍生反应30min，正己烷定容后进样分析，外标法定量。本方法氯霉素在1.0～500．0μg／L，氟甲砜霉素和甲砜霉素在5．0～500．0μg/L浓度范围内呈线性相关，相关系数r≥0．9983，加标水平在0．2～10．0μg/kg时，回收率为83.30％～101．22％，相对标准偏差为1．36％～12．57％。氯霉素、氟甲砜霉素和甲砜霉素的检测限分别为0．1、0．2、0．2μg/kg。

A capillary gas chromatography with electron capture detection method was developed for determining the residues of chloramphenicol, florfenicol, and thiamphenicol in fishery products. Sample were extracted with ethyl acetate, the extracts were evaporated to dryness and then the residues were dissolved in methanoL/NaCl water solution, defatted with hexane, and passed through a C18 SPE column. The SPE column was eluted with acetonitrile. The elute was derivatized with BSTFA-TMCS The derivatization solution was evaporated to dryness, followed by hexane dissolve the derivatization, the samples were ready for determination. Using external stand quantitation. The standard curves were linear in the investigated ranges, 1.0 - 500. 0 μg/L of chloramphenicol and 5 - 500. 0μg/L of florfenicol and thiamphenicol. The correlation coefficient r≥0. 9983. The recoveries were 83.30% - 101.22% at spiking levels 0, 2 - 10. 0 μg/kg. The relative standard deviations were 1.36% - 12. 57%. The detection limit of chloramphenicol, florfenicol, and thiamphenicol were 0. 1, 0. 2, 0.2 μg/kg respectively.