摘要
建立了黄瓜和番茄中毒氟磷残留量的固相翠取-气相色谱-质谱联用（SPE-GC-MS）分析方法;对毒氟磷的裂解机理进行了探讨，确定了测试分析的定性离子和定量离子。样品采用V（正己烷）： V（丙酮）=1：1混合液高速匀浆提取，使用以N-丙基乙二胺（PSA）, C18和石墨化炭黑（GCB）的混合物为填料的固相翠取柱净化，采用气相色谱-质谱联用仪在选择离子扫描（SIM）模式下进行检测，外标法定量。结果显示，毒氟磷在0. O1-0.5 mg/L内，标准溶液的峰面积与质量浓度的线性关系良好（r ≥0. 999 ），方法的检出限（LOD）（S/N=3）为0.003 mg/kg，定量限（LOQ）（S/N =10）为0.01 mg/kg。在0.01, 0.02和0. 1 mg/kg添加水平下，毒氟磷的平均回收率为99.9%-100.2%，相对标准偏差（RSD,n=6）为0.97%-3.07%.
A solid phase extraction coupled with gas chromatography-mass spectrometric （SPE-GC- MS） method was established for the determination of Dufulin residue in cucumber and tomato. After extracted with V（n-hexane） ： V（acetone） = 1： 1 mixture in high-speed homogenized extract method, the target samples were cleaned up in solid phase extraction by the mixture of N-propylethylenediamine （PSA）, C18 and graphitized carbon （GCB）, analyzed by GC-MS under selected ion monitor mode （SIM） and quantified by the external standard method. Good linear between the peak area and the concentration of Dufulin was obtained in the range of 0.01 - 0.5 mg/L with correlation coefficient not less than 0.999 under the optimum conditions, the limit of detection （LOD） （ S/N = 3 ） was 0. 003 mg/kg and the limit of quantitation （LOQ） （SIN = 10 ） was 0.01 mg/kg. The average recoveries of Dufulin from the cucumber and tomato blank samples at three spiked levels of 0.01,0.02 and 0. 1 mg/kg ranged from 99.9% to 100.2% with RSD of 0.97% - 3.07%. The fragmentation mechanism of Dufulin was also studied in which the qualitative ions and quantitative ions were confirmed.
出处
《农药学学报》
CAS
CSCD
北大核心
2013年第5期523-527,共5页
Chinese Journal of Pesticide Science
基金
福建出入境检验检疫局科技项目(FK2012-16)
关键词
固相萃取-气相色谱-质谱联用
黄瓜
番茄
毒氟磷
裂解机理
solid phase extraction-gas chromatography-mass spectrometry （ SPE-GC-MS ）
cucumber
tomato
Dufulin
fragmentation mechanism
作者简介
丁立平，通信作者（Author for correspondence），男，工程师，硕士，从事进出口食品有害物质检测工作，E-mail：43548624@qq．com
