滩涂及贝类中残留三唑磷的GC/MS分析  

Determination of triazophos residues in shoal mud and shoal shells by GC/MS

作　　者：徐继林[1] 严小军[1] 王国良[1] 薛超波[1] 

机构地区：[1]宁波大学生命科学与生物工程学院,浙江宁波315211

出　　处：《海洋环境科学》2004年第4期53-56,共4页Marine Environmental Science

基　　金：国家新药基金项目(2003AA2Z3511)宁波市科技局项目(01N40100-74)

摘　　要：建立了滩涂和贝类中残留有机磷类农药三唑磷的毛细管气相色谱-质谱联用检测法.向冷冻干燥后的样品中加入邻苯二甲酸二戊酯作为定量内标物,用乙酸乙酯:正己烷(体积分数1:1)提取,浓缩定容后用EI源在SIM检测模式下进行检测.结果表明,三唑磷与内标物在SBP-50柱上得到良好的分离,色谱峰尖锐,没有杂峰干扰.在(2.50～50.00)ng/mL浓度范围内具有良好的线性关系,线性方程为y=8.261×10-4x,相关系数为0.999 8.方法的最低检测限0.18×10-9.平均回收率为90.96%～102.15%,相对标准偏差为3.81%～4.82%.对采自浙江沿海7个采样点沉积物和三种海产贝类进行了测定,三唑磷含量在(0～1.31)×10-6范围内.A sensitive analytical method on triazophos residues in shoal mud and shells was established with capillary gas chromatography - mass spectrometry. The triazophos in the mud samples and shell muscle samples can be extracted with ethyl acetate : n-hexane (1:1 V/V) effectively, and determined using EI-SIM-MS after concentration. The results shown that triazophos and the inner standard can be separated each other on SBP-50 column, with sharp peak and rare contamination. The linearity is superior from 2.50 to 50.00 ng/mL, with the lowest detection limit of 0.18 × 10-9. The average recovery rate is 90.96 - 102.15% respectively, after spiking triazophos 10.00 - 500.00 × 10-9 into 5.00 g sample. The standard deviation ranges from 3.81 % to 4.82 %. This method is applied to determine the triazophos residues in different marine shoal mud and three shell species samples from 7 places with the results of 0 - 1.31 × 10' .

关 键 词：滩涂 贝类 三唑磷 气相色谱质谱联用 

分 类 号：O657.7[理学—分析化学] X592[理学—化学]