摘要
为建立动物组织中氟苯尼考残留量测定的可靠、灵敏的气相色谱-质谱联用分析方法.采用乙腈提取猪肉组织试样,经C18固相小柱净化,用体积分数为60%甲醇水溶液洗脱,吹干,用Sylon BFT在50℃衍生20min后,进行检测.采用选择离子监测(m/z178、257、259)模式进行定性定量分析测定,衍生物SIM的总离子流图峰面积与试样质量浓度在5.00～1000.00μg/L范围内呈良好的线性关系,线性回归系数大于0.999,方法最低检出限达2.0μg/kg.猪肉组织在1.0、10.0和100.0μg/kg三水平加标平均回收率分别为88.4%、84.0%和71.2%,相应的变异系数分别为8.7%、6.8%和11.5%.同时,对氟苯尼考三甲基硅醚衍生物的EI质谱可能裂解途径进行了解析.
The objective of the present study was to develop a reproducible, sensitive method to determine florfenicol residues in pork by GC-MS. The composite samples were extracted with acetonitrile, and purified with a C_(18) cartridge successively. The drug was eluted from the cartridge with 60% (φ) methanol water solution. After toluene and Sylon~ BFT were added to the residues, the drug was derivatived at 50 ℃ for 20 min, and more toluene was added and then applied to GC-MS. SIM mode was performed at m/z 178, 257 and 259. The range of linearity was 5.00-(1 000.00) μg/L, the relevant coefficient was more than 0.999, and the lowest detection limit of the method was 2.0 μg/kg. Recoveries from porks fortified at 1.0, 10.0 and 100.0 (μg/kg) were 88.4%, 84.0% and 71.2%, respectively, and the corresponding RSDs were 8.7%, 6.8% and 11.5%, respectively. Meanwhile, the fragmentation pathways of main fragment ions of TMS derivative of florfenicol was interpreted.
出处
《华南农业大学学报》
CAS
CSCD
北大核心
2005年第3期100-102,共3页
Journal of South China Agricultural University
基金
国家科技攻关计划子课题(2002BA906A7501)
