食品科学 ›› 2008, Vol. 29 ›› Issue (11): 562-566.

• 分析检测 • 上一篇    下一篇

微波辅助萃取-气相色谱法测定茶叶中多种有机氯和拟除虫菊酯农药残留

 曾小星, 万益群, 谢明勇   

  1. 南昌大学食品科学与技术国家重点实验室; 南昌大学分析测试中心;
  • 出版日期:2008-11-15 发布日期:2011-12-08

Determination of Organochlorines and Pyrethroids Residues in Tea from Jiangxi Province with Microwave-Assisted Extraction-Gas Chromatography

 ZENG  Xiao-Xing, WAN  Yi-Qun, XIE  Ming-Yong   

  1. 1.State Key Laboratory of Food Science and Technology,Nanchang University,Nanchang 330047,China;2.Center of Analysis and Testing,Nanchang University,Nanchang 330047,China
  • Online:2008-11-15 Published:2011-12-08

摘要: 建立了茶叶中18种有机氯和9种拟除虫菊酯农药残留微波辅助萃取-气相色谱分析方法。运用正交设计法对微波萃取条件进行了优化,茶叶样品用正己烷-二氯甲烷混合溶剂(1:2,V/V)进行萃取,萃取液用弗罗里硅土和中性氧化铝混合层析柱净化,采用J&WDB-1701毛细管柱分离,GC-ECD法同时测定。在0.4、0.2、0.1ml(0.5μg/ml有机氯农药+1.0μg/ml拟除虫菊酯农药)三个水平添加时的平均回收率(n=5)分别为80.9%~118.5%、88.4%~120.7%、80.9%~116.3%;相对标准偏差分别为2.09%~6.70%、1.89%~6.49%、1.98%~11.87%。该方法的检出限为:有机氯农药0.0004~0.0048mg/kg,拟除虫菊酯农药0.0033~0.0400mg/kg。

关键词: 茶叶, 有机氯农药, 拟除虫菊酯农药, 微波辅助萃取, GC-ECD

Abstract: A new method for multiresidue analysis of 18 organochlorines and 9 pyrethroids in tea from Jiangxi province was established.The pesticide residues were extracted from tea samples with hexane-dichloromethane(1:2,V/V) by using microwave-assisted methed,and the microwave-assisted extraction conditions,such as the extraction solvent type,volume,microwave heating time and microwave temperature were optimized with orthogonal test design.The extracts were purified with alumina neutral-florisil column,and then determined with gas chromatography equipped with electron-capture detector(GC-ECD),using DB-1701 capillary column.The recoveries obtained from Chinese tea samples(n=5) added with pesticide standards at the three levels of 0.4,0.2 and 0.1ml(0.5 μg/ml organochlorines plus 1.0 μg/ml pyrethroids) are in the ranges of 80.9% to 118.5%,88.4% to 120.7% and 80.9% to 116.3% with the RSDs in the ranges of 2.09% to 6.70%,1.89% to 6.49% and 1.98% to 11.87%,respectively.The detection limits of the organochlorine pesticides are in the range of 0.0004 to 0.0015 mg/kg,and those of the pyrethroids are in the range of 0.0067 to 0.0365 mg/kg.

Key words: tea, organochlorine pesticides, pyrethroid pesticides, microwave-assisted extraction, GC-ECD