高效液相色谱-串联质谱法同时测定农田土壤中31种三嗪类除草剂残留

Determination of 31 Triazine Herbicides in Farmland Soils by High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立了高效液相色谱-三重四极杆串联质谱（HPLC-MS/MS）同时检测农田土壤中31种三嗪类除草剂残留的分析方法.土壤样本经加速溶剂萃取,Oasis MCX固相萃取柱净化后,在多反应监测（MRM）正离子电喷雾模式下进行HPLC-MS/MS分析.色谱柱为Phenomenex Luna C18反相柱（150mm＆#215;2.0 mm＆#215;3μm）,流动相为梯度变化的乙腈和0.1％甲酸溶液.检出限（S/N≥3）为0.008～0.440 μg/L,在各自的考察浓度范围内线性关系良好（r≥0.996）;在0.40 ～ 40.0 μg/kg添加水平内,平均加标回收率为76.9％～102.0％,RSD为3.4％～10.3％.利用本方法对沈阳地区农田表土的筛查发现,阿特拉津、西玛津、扑草净和脱乙基阿特拉津为该区域主要的三嗪类除草剂物种.

A high performance liquid chromatography-tandem mass spectrometric method （HPLC-MS/MS） was developed for the simultaneous determination of 31 kinds of triazine herbicides in farmland soils. Samples were extracted by accelerated solvent extraction （ASE） and purified by Oasis MCX solid phase extraction （SPE） cartridges, and then analyzed by HPLC-MS/MS in multiple reaction monitoring （MRM） mode with positive electrospray ionization. The analytical column was Phenomenex Luna C18 （ 150 mm × 2.0 mm × 3 μm） and the mobile phases were acetonitrile and water containing 0.1% （V/V） formic acid. The limits of detection （ S/N≥3 ） were 0.008-0. 440 μg/L. All of the triazine herbicides had good linear responses with r≥0. 996 and the average recoveries in the spiked levels of 0.40-40.0 μ,/kg ranged from 76.9%-102.0% with the RSDs of 3.4%-10.3%. The HPLC-MS/MS method had been applied for the detection of the triazine herbicide residues in farmland soils from Shenyang region and the results showed that atrazine, simazine, prometryne and atrazine-desethyl were the main triazine herbicides in the region.