摘要
建立了柱层析法/气相色谱(GC)-负化学离子源(NCI)质谱检测牛肉中7种常用拟除虫菊酯杀虫剂残留的方法。样品经乙腈提取,通过中性氧化铝层析柱净化后,再由气相色谱-负化学离子源质谱选择离子监测技术(SIM)进行测定。7种菊酯类农药标准溶液在10~1000μg/L范围内线性关系良好,r^2均大于0.997。在10、20、50Ixg/kg加标水平下的回收率为80%~108%,相对标准偏差(RsD)不高于12.5%。结果表明,方法的选择性高,分离效果好,其检出限(LOD)为0.10—2.5μg/kg,定量下限(LOQ)为0.50—5.0μg/kg。
A gas chromatography ( GC ) - negative chemical ionization - mass spectrometric ( NCI/ MS ) method was established for the determination of 7 frequently used pyrethroid insecticides residues in beef. The sample was extracted with acetonitriles and cleaned up with neutral alumina chromatographic column, and then determined by GC - MS under the selected ion monitoring mode (SIM). Good accuracy, precision and sensitivity were obtained. The calibration curves of 7 pyrethriods were linear between peak areas'and concentrations in the range of 10 - 1 000μg/L with correlation coefficients(r2) more than 0. 997. The recoveries of 7 pyrethriods were in the range of 80% -108% at three spiked concentration levels of 10, 20, 50 μg/kg, with relative standard deviations (RSDs) less than 12.5%. The limits of deteetion(LOD) for all pyrethroid ranged from 0. 10 μg/kg to 2. 5 p,g/kg and the limits of quantitation(LOQ) were in the range of 0. 50 -5.0 μg/kg.
出处
《分析测试学报》
CAS
CSCD
北大核心
2011年第3期316-320,共5页
Journal of Instrumental Analysis
基金
2009年农业行业标准制定项目
关键词
气相色谱-负化学离子源质谱
柱层析
选择离子监测
拟除虫菊酯
牛肉
gas chromatography- negative chemical ionization mass spectrometry
column chromatography
selected ion monitoring
pyrethroid
beef