摘要
建立了SPE-HPLC-MS法定量测定果蔬中农药马拉硫磷残留量。固相萃取小柱为SupelcleanTM ENVITM-18柱（3 mL）,丙酮为洗脱液;色谱柱为安捷伦快速高分离亚二微米液相色谱柱Zorbax RRHTSB-C18（1.8μm,4.6 mmi.d.×50mm,Agilent）;流动相为70%甲醇（含2 mmoL甲酸铵）＋30%水,等梯度洗脱;质谱采用正离子电离方式,选择m/z 283和m/z 243碎片离子为定性离子,以丰度最高的碎片离子m/z 283为定量离子,用MRM模式监测;外标法定量。方法相关系数r2=0.9968,检出限（LOD）为0.002 mg/kg,加标回收率为78.3%-96.2%,相对标准偏差（RSD）为3.5%-18.8%,适合样品中低含量马拉硫磷残留量的测定。
A SPE-HPLC-MS method has been developed for the determination of pesticide malathion residue in garden spgarden stuff quantificationally with SPE as the pre-processing method of sample, HPLC as the separating means and MS as the quantitative detector. Its quantitative basis is in terms of the liner relationship between the concentration and the peak area of the ion current chromatogram of monitored ion. The SPE pillaret was Supelclean^TM ENVI^TM-18 （3 mL） ; the eluent was acetone; the chromatographic column was zorbax RRHT SB - C18 （ 1.8 μm, 4.6 × 50 mm, Agilent） ; the mobile phase was 70% methanol （containing 2 mmoL ammonium formate） ＋ 30% H2O. Mass spectrometry was operated in the positive ion mode. The fragment ions m/z 283 and 243 were selected for qualitative analysis, and the most abundant fragment ion m/z 283 was chosen for quantification. The good linearity was obtained in the range of 0. 02 -4.0 mg/L with the correlation coefficient （r^2） of 0. 9968; the limit of detection was 0.002 mg/kg; the recoveries were 78.3% -96.2% at the spiked levels of 0.02, 2.0 and 4.0 mg/L with the relative standard deviations of 3.5- 18.8%.
出处
《分析试验室》
CAS
CSCD
北大核心
2008年第10期10-14,共5页
Chinese Journal of Analysis Laboratory
基金
黑龙江省教育厅(11511082)项目资助
