摘要
建立了大豆和玉米中苯甲酰脲类农药的反相高效液相色谱-电喷雾串联质谱(LC-ESIMS/MS)检测方法。样品经含0.1%乙酸的乙腈提取、浓缩,阳离子固相萃取柱净化,液相色谱串联质谱测定。9种苯甲酰脲类农药在5.0～200μg/L范围内线性关系良好(r2>0.995)。在大豆和玉米基质中的检出限均为3.0μg/kg,定量下限均为10.0μg/kg。在10.0、20.0、50.0μg/kg 3个加标水平下,9种苯甲酰脲类农药的回收率为46%～92%,精密度(RSD)小于14%。方法准确、灵敏、简单,适用于大豆和玉米中9种苯甲酰脲类农药残留的同时测定。
A high performance liquid chromatography - mass spectrometric （ HPLC - MS） method was developed for the determination of benzoylurea insecticides residues in soya beans and corns. The sample was extracted by acetonitrile containing 0. 1% acetic acid and cleaned up by solid-phase extraction. The extract was analyzed by reversed-phase HPLC -ESI MS/MS. The calibration curves showed good linearities in the range of 5.0 -200. 0 μg/L with correlative coefficients more than 0. 995. The limits of detection（LOD） for 9 benzoylurea insecticides from soya beans and corns matriex were 3.0 μg/kg and the limits of quantitation（LOQ） were 10.0 μg/kg. The spiked recoveries of 9 benzoylurea insecticides at three concentration levels of 10.0, 20. 0 and 50. 0 μg/kg ranged from 46% to 92% with RSDs less than 14%. The method established was accurate, sensitive and simple, and was suitable for the simultaneous analysis of benzoylurea insecticides residues in soya beans and corns.
出处
《分析测试学报》
CAS
CSCD
北大核心
2010年第11期1180-1184,共5页
Journal of Instrumental Analysis
关键词
液相色谱-质谱联用
苯甲酰脲类农药
大豆
玉米
liquid chromatography - mass spectrometry （ LC - MS）
benzoylurea insecticide
soya bean
corn
