牛奶中有机氯农药及拟除虫菊酯农药多残留的HS-SPME-GC-MS分析方法研究  

Headspace Solid-Phase Microextraction Combined with Gas Chromatography Mass Spectrometry for Determination of Organochlorine and Pyrethroid Pesticides in Milk

作　　者：朱捷[1] 杨欣[2] 封锦芳[3] 施志雄[2] 赵云峰[2] 周艳明[1] 吴永宁[2] 

机构地区：[1]沈阳农业大学食品科学院,辽宁沈阳110161 [2]中国疾病预防控制中心营养与食品安全所,北京100050 [3]首都医学科大学公共卫生与家庭医学院,北京100069

出　　处：《中国食品卫生杂志》2007年第4期289-293,共5页Chinese Journal of Food Hygiene

基　　金：国家"十五"科技攻关重大项目<食品安全关键技术研究>重要有机污染物痕量与超痕量检测技术的研究(2001BA804A19和2001BA804A45)

摘　　要：目的建立牛奶中有机氯农药和拟除虫菊酯类农药的快速多残留测定方法。方法以顶空固相微萃取作为前处理手段,采用气相色谱-质谱联用方法测定牛奶样品中31种农药组分(其中有机氯农药23种,拟除虫菊酯类农药8种),并以13C6-六氯苯和13C10-灭蚁灵作为稳定的同位素内标物,采用内标法定量。结果方法的最低检测限在0.002～0.2μg/L之间,回收率在85%～110%之间,相对标准差在3%～12%之间。结论该方法快速、简单、准确、可靠、环保。适用于批量牛奶样品中农药残留的筛查。Objective A rapid method was developed for multi-residues determination of organochlorine and pyrethroids pesticides. Method Headspace solid-phase microextraction （HS-SPME） was used as sample pretreatment method for extraction and concentration. Gas chromatography with mass spectrometry detection （GC-MSD） was used to analyze 31 pesticides （included 23 organochlorine pesticides and 8 pyrethroids） in milk. Two stable isotope compounds, 73 C6 labeled hexachlorobenzene and t3 C^0 labeled mirex, were used as internal standards for the quantification. Results The method showed good recoveries （range from 85% to 110%） and repeatability （RSD 〈 12%） for all compounds, with detection limits ranging from 0.002 to 0.2 μg/L. Conclusion As the analytical procedure does not include any concentration or cleanup steps, it is easy and fast to perform, making it applicable for analysis in pesticides monitoring programmes in milk.

关 键 词：除虫菊酯类 农药 烃类 氯化 碎片质谱法 化学 分析 乳 

分 类 号：R155.5[医药卫生—营养与食品卫生学]