GC-MS测定土壤中阿特拉津、六氯苯等十种农药残留

建立了气相色谱-质谱-选择离子监测(GC-MS-SIM)同时测定土壤中10种农药(三嗪类除草剂、酰胺类除草剂和有机氯农药)的多残留分析方法.样品采用正己烷/丙酮(1:1,V/V)超声提取、氟罗里硅土柱层析净化、GC-MS-SIM测定.10种农药在0.01(0.02)-1.0(2.0)mg·l~(-1)范围内线性良好,相关系数介于0.9963-0.9998之间;在10,50和250 ng·g~(-1)添加水平下,平均回收率介于81%-117%之间,相对标准偏差均小于14.4%;方法检出限达到ppb至sub-ppb级(0.1-1.3 ng·g~(-1)).将此方法应用于辽宁省不同性质土壤中70个实际土壤样品的分析,阿特拉津、乙草胺、六氯苯、丁草胺、狄氏剂和艾氏剂有检出,该法对不同性质土壤具有广泛适用性.

SIMULTANEOUS DETERMINATION OF 10 HERBICIDES AND ORGANOCHLORINE PESTICIDES IN SOIL BY GC-MS

A gas chromatography-mass spectrometry-selected ion monitoring(GC-MS-SIM) method has been developed for multi-residue analysis of 10 pesticides (triazine herbicides, chloroacetanilide herbicides and organochlorine pesticides) in soil. The method is based on ultrasonic extraction using hexane/acetone (1: 1, V/V), florisil cleanup and GC-MS-SIM determination. The linear ranges of the 10 pesticides were 0.01 (0.02) 1.0 (2.0) mg·l~(-1), and the correlation coefficients were 0.9963-0.9998. The average recoveries of the 10 pesticides at the three spiked levels(10, 50, 250 ng · g~(-1)) ranged from 81% to 117% with good precision (< 14.4%) . Pesticides residues could be detected in the low- to sub-ppb range (0.1-1.3 ng · g~(-1)) . This methodology has been applied to analysis of 70 real soil samples of different characteristics from Liaoning Province in which atrazine, acetochlor, hexachlorobenzene, butachlor, dieldrin and aldrin were detected. It is widely applicable for soil of different properties.