摘要
采用响应面法(RSM)优化了烟草中有机氯农药残留的加速溶剂萃取(ASE)条件,并利用气相色谱-质谱法进行定性定量分析。以有机氯农药平均回收率为指标,考察了加速溶剂萃取过程中提取溶剂、萃取温度、冲洗溶剂体积、循环次数和吹扫时间等因素对烟草中有机氯提取效果的影响。经响应面优化的最佳ASE条件为:提取溶剂为正己烷-丙酮(体积比9:1),萃取温度107℃,冲洗体积92%,吹扫时间92s,循环次数3次。在优化条件下,烟草有机氯农药萃取回收率理论预测值为96.5%,验证值为94.9%。结果表明,响应面法适用于烟草中有机氯农药残留加速溶剂萃取条件的优化,经优化得到的萃取参数准确可靠,具有实用价值。
Response surface methodology(RSM) was used to optimize experimental conditions of accel- erated solvent extraction(ASE) for organochlorine pesticide (OCPs) residues in tobacco. The qualita- tive and quantitative analysis was performed by gas chromatography -mass spectrometry. The average recovery of OCPs was selected as the index for evaluation of the effect of extraction solvent, extraction temperature, flush volume and purge cycle time on the extraction efficiency of organochlorine in to- bacco. The best extraction conditions of accelerated solvent extraction determined by response surface optimization were as follows : extraction solvent : n-hexane - acetone (9 : 1, by volume) solution, extraction temperature: 107 ~C, flush volume: 92% , purge time: 92 s, cycle number: 3 times. Under the optimized conditions, the average recovery of OCPs was 96. 5% (theoretical) or 94. 9% (actual). The results showed that the application of RSM for the optimization of ASE conditions for organoehlorine pesticide residues in tobacco was feasible, and the parameters optimized by RSM were accurate, reliable, and have practical value.
出处
《分析测试学报》
CAS
CSCD
北大核心
2009年第9期1012-1017,共6页
Journal of Instrumental Analysis
关键词
响应面法
有机氯农药残留
加速溶剂萃取
气相色谱-质谱联用
烟草
response surface methodology
organoehlorine pesticides residue
accelerated solvent extraction
GC - MS
tobacco