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建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)测定土壤、沉积物和水中溴嘧氯草醚残留量的方法,研究了溴嘧氯草醚在3种不同类型土壤中的降解特性。样品经乙腈提取后,以C_(18)固相萃取柱净化,采用梯度洗脱程序、BEH C_(18)色谱分离柱、应用UPLC-MS/MS多反应监测模式测定溴嘧氯草醚。对0.005、0.05和2.0 mg/kg添加浓度样品进行回收实验,溴嘧氯草醚在土壤、沉积物和水中的平均回收率为87%~106%,变异系数为2.8%~8.0%。溴嘧氯草醚在0.5~20μg/L浓度范围内相关系数R~2>0.9999,溴嘧氯草醚在土壤(沉积物)和水中的定量限分别为0.2μg/kg和0.2μg/L。应用建立的溴嘧氯草醚残留分析方法检测了土壤降解样品,结果表明,溴嘧氯草醚在3种不同土壤中好氧降解的半衰期为1.72~28.2 d,厌氧降解的半衰期为2.93~31.4 d;在同一种土壤样品中,好氧条件下溴嘧氯草醚降解快于厌氧条件;土壤中溴嘧氯草醚降解的快慢与土壤的pH值、阳离子交换量和土壤质地有关。
A method for the determination of bromothiazinol in soils, sediments and water by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) has been established. The effects of bromoxynil in three different soil types Degradation characteristics. The samples were extracted with acetonitrile and purified with C 18 solid phase extraction column. The gradient elution program and BEH C 18 chromatography were used to determine the concentrations of bromoxynil by UPLC-MS / MS. The average recoveries of bromoxynil in soils, sediments and water ranged from 87% to 106%, and the coefficients of variation were from 2.8% to 8.0% for the recoveries of 0.005, 0.05 and 2.0 mg / kg. The correlation coefficient of bromoxynil in the range of 0.5 ~ 20μg / L was R ~ 2> 0.9999, and the limit of quantification of bromoxynil in soil (sediment) and water was 0.2μg / kg and 0.2μg / L, respectively. The results showed that the half-life of bromoxydine in aerobic degradation of three different soils was 1.72 ~ 28.2 d, the half-life of anaerobic degradation was 2.93 ~ 31.4 d. In the same soil samples, the degradation rate of bromopyrimidone was faster than anaerobic conditions in aerobic conditions. The degradation rate of bromoxydine in soil was related to soil pH value, cation exchange capacity and soil texture.