论文部分内容阅读
利用串联质谱正负离子切换模式功能,建立了一种能快速同时检测农田土壤中2,4-二氯苯氧乙酸,敌稗和二嗪磷残留的液相色谱-串联质谱(HPLCM S/M S)分析方法。样品以加速溶剂萃取,Supelclean ENVI-18固相萃取柱净化,多反应监测(MRM)正负离子切换电喷雾模式进行分析。色谱柱为Luna C18柱(150 mm×2.0 mm,3μm),流动相为梯度变化的5 mmol/L甲酸铵甲醇溶液和5 mmol/L甲酸铵水溶液。方法检出限(S/N≥3)介于0.94~8.35 ng/L,相关系数≥0.999;在1.0~10.0μg/kg添加水平内,平均加标回收率介于73.8%~106.9%之间,RSD介于5.8%~11%。利用该方法对某地区农田表土的筛查发现该地区存在二嗪磷使用历史,但污染程度较轻。
A tandem mass spectrometry (HPLC-MS / MS) method was developed for rapid and simultaneous determination of 2,4-dichlorophenoxyacetic acid, propanil and diazinon residues in agricultural soils by tandem mass spectrometry (tandem mass spectrometry) Analytical method. The samples were analyzed by accelerated solvent extraction, Supelclean ENVI-18 cartridge purification and MRM positive and negative ion-exchange electrospray mode. The column was a Luna C18 column (150 mm × 2.0 mm, 3 μm). The mobile phase consisted of a gradient of 5 mmol / L ammonium formate methanol and 5 mmol / L ammonium formate. The detection limits (S / N≥3) ranged from 0.94 to 8.35 ng / L with the correlation coefficients ≥0.999. The mean spike recoveries ranged from 73.8% to 106.9% at 1.0 ~ 10.0 μg / kg , RSD ranged from 5.8% to 11%. Using this method to screen the topsoil of arable land in a certain area, we found that diazinon use history exists in this area, but the degree of pollution is light.