摘要
目的：建立海洋滩涂沉积物环境中三唑磷残留的毛细管气相色谱-质谱联用检测法。方法：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，用乙酸乙酯：正己烷（1：1v／v）提取，浓缩定容后用EI源在SIN检测模式下进行检测。结果：三唑磷与内标在SBP-50柱上得到良好的分离，色谱出峰尖锐，没有杂峰干扰。方法在2．50-50．00ng／ml浓度范围内线性关系良好，线性方程为Y：8．261×10^-4X，相关系数为0．9998。最低检测限为0．27ng／g。当向5．00g样品中添加三唑磷10．00—500．00ng／g时，平均回收率达到90．96％-102．15％，标准相对偏差为3．81％-4．82％。结论：宁波沿海滩涂沉积物环境中三唑磷残留量为0．061—0．078mg／kg。
Objective： To establish a sensitive analytical method for detection of triazophos residues in marine shoal mud using capillary gas chromatography - mass spectrometry. Methods：The triazophos in the mud samples were extracted with ethyl acetate ： n - hexane （ 1 ： 1 v/v） effectively, and determined using EI - SIM - MS after concentration. Results： Triazophos and the inner standard can be separated from each other on SBP -50 column,with sharp peak and rare contamination. The linearity was superior from 2. 50 to 50. 00 ng/ml ,with low detection limit of 0. 27 ng/g. The average recovery rate was 90. 96% - 102. 15% after spiking triazophos 10. 00 -500. 00 ng/g into 5. 00 g sample. The standard deviation ranged from 3.81% to 4. 82%. Conclusion：The triasophos residues in different marine shoal mud are 0. 061 - 0. 078 mg/g.
出处
《中国卫生检验杂志》
CAS
2006年第5期522-523,618,共3页
Chinese Journal of Health Laboratory Technology
基金
宁波市科技局项目(01N40100-74)
