顶空-固相微萃取-气相色谱法测定甘蔗中的莠去津  

Determination of atrazine in sugar cane by headspace solid phase micro-extraction coupled with gas chromatography

作　　者：郭和光[1] 吴丹青[1] 邵国健[1] 姚建花[1] 

机构地区：[1]湖州市疾病预防控制中心理化科,浙江湖州313000

出　　处：《中国卫生检验杂志》2016年第18期2614-2615,2619,共3页Chinese Journal of Health Laboratory Technology

基　　金：浙江省湖州市计划项目(2015GYB14)

摘　　要：目的建立顶空-固相微萃取-气相色谱法测定甘蔗中莠去津残留量的方法。方法称取混匀样品于10 ml顶空瓶中,加入乙酸盐缓冲液及氯化钠溶液,50℃搅拌预热2 min,用聚二甲基硅氧烷萃取头(PDMS,100μm)在500 r/min搅拌下顶空萃取20 min,在280℃进样口解吸3.0 min,用HP-INNOWAX毛细管色谱柱分离,ECD检测器检测甘蔗中莠去津的残留量。结果莠去津的浓度为0.005μg/g^0.20μg/g时,线性关系良好,相关系数(r)=0.999 6,方法的检出限为0.000 06 mg/kg,平均回收率为95.8%~98.6%,相对标准偏差(RSD)为2.3%~4.9%。结论顶空-固相微萃取-气相色谱法测定甘蔗中莠去津残留量的方法,无需有机溶剂,集萃取分离、浓缩净化、解吸、进样等过程于一体,具有环保、操作简便、快速、基质干扰少、灵敏度高、测定范围宽,分析结果准确可靠,适用于甘蔗样品中莠去津残留量的测定。Objective To establish a method for the detection of atrazine residues in sugar cane by headspace solid phase micro-extraction coupled with gas chromatography. Methods To weigh well- mixing samples in 10 ml headspace bottle,add in acetate buffer and sodium chloride solution,then stir and warm up at 50 ℃ for 2 min,stir and extract headspace sample with polydimethylsiloxane extraction head（ PDMS,100 μm） for 20 min at 500 r / min,and desorp samples at 280 ℃ for 3. 0 min.After separating out by HP- INNOWAX capillary chromatogram column,to test the atrazine residue in sugar cane with ECD detector. Results Good linearity was obtained when concentration of atrazine was within 0. 005 μg / g- 0. 20 μg / g,with the correlation coefficient（ r） of 0. 9996,the method detection limit was 0. 000 06 mg / kg,the average recovery rate was within95. 8%- 98. 6%,with relative standard deviation（ RSD） of 2. 3%- 4. 9%. Conclusion The method for the detection of atrazine in sugar cane by headspace solid phase micro- extraction coupled with gas chromatography needs no organic solvent,extraction,separation,concentration,purification,desorption and sampling. It is environmentally safe,convenient and quick with less matrix interference,high sensitivity,wide measurement range,accurate and reliable analytic result. It applies to the determination of atrazine residues in sugar cane.

关 键 词：莠去津 甘蔗 顶空固相微萃取 气相色谱法 

分 类 号：O657.71[理学—分析化学]