摘要
建立了液液提取-固相萃取-气相色谱火焰光度法(LLE-SPE-GC-FPD)测定牛肉中蝇毒磷的残留量。优化了气相色谱分离条件,研究了样品基质对蝇毒磷测定的影响,考察了Florisil固相萃取小柱和ODS固相萃取小柱的萃取效果,并选择乙酸乙酯为洗脱剂,考察了液-液提取和固相萃取的回收率。将该方法用于牛肉中蝇毒磷的测定,其检出限为0.02μg/mL,回收率高于83%,相对标准偏差13.7%。使用气相色谱质谱仪(GC-MS)对样品中的蝇毒磷进行定性分析,其特征离子和相对丰度为362(100)、226(55)和210(40)。
A method was studied for the analysis of comnaphos residue in beef by using liquid liquid extraction-solid phase extraction-gas chromatography with flame photometric detector （LLE-SPE-GC-FPD）. The conditions of separation for gas chromatography was optimized, the effect of sample matrix on coumaphos was studied in detail, and the extraction efflciency of Florisil SPE column and ODS SPE column for coumaphos was reviewed. The ethyl acetate was selected as eluent in comparison with acetone, the recovery of liquid-liquid extraction and solid phase extraction was examined. The developed method was applied to the detertnination of coumaphos in beef, the limit of detection （LOD） of this method is lower than 0.02 μg/g, the recovery is above 83%, and the relative standard deviation （RSD） 13.7%. The results are satisfactory. The coumaphos was identified by gas chromatography-mass spectrometry （GC- MS）, the diagnostic ions and the relative abundance in the mass spectra are 362（ 100）, 226（55） and 210（40）.
出处
《分析试验室》
CAS
CSCD
北大核心
2007年第10期5-8,共4页
Chinese Journal of Analysis Laboratory
基金
农业部农业行业标准基金资助项目(农财发[2005]58号250)
关键词
蝇毒磷
固相萃取
气相色谱
牛肉
Coumaphos
Solid phase extraction
Gas chromatography
Beef
