超高液相色谱串联质谱法测定养殖水体中三唑磷

Determination of Triazophos in Aquaculture Water by UPLC- MS / MS

[目的]研究超高液相色谱串联质谱法测定养殖水体中三唑磷的可行性。[方法]建立了超高效液相色谱串联质谱法测定养殖水体中三唑磷的分离方法。采用二氯甲烷和正己烷分次提取合并,用碱性氧化铝柱净化样品,以外标法定量。分别对淡水和海水进行低、中、高(1.0、5.0、25.0 ng)3个梯度浓度进行加标,并测定其回收率。[结果]超高液相色谱串联质谱法的标准液浓度为1.0~60.0μg/L时,线性良好(R^2=0.999 0),回收率为78.3%~88.3%,RSD为4.39%~7.56%,方法检出限在0.002μg/L。[结论]超高液相色谱串联质谱法灵敏度高,检测速度快的特点,可用于养殖水体中三唑磷的检测分析。

[Objective] To research determination feasibility of triazophos in aquaculture water by UPLC-MS / MS.[Method]Isolation method for triazophos determination in aquaculture water was established by UPLC-MS / MS. Dichloromethane and hexane were used to extract samples,respectively. Then,we combined the extracted liquid and purified the samples by basic alumina column. External standard method was used for quantification. Standard was added in three gradient concentrations（ 1. 0,5. 0,25. 0 ng） in freshwater and seawater. And the recovery rate was detected.[Conclusion] When the concentration of standard solution was 1. 0- 60. 0 μg / L,the linearity was good（ R^2= 0. 999 0） and the recovery rate was 78. 3%- 88. 3% and RSD was 4. 39%- 7. 56%. Method detection limit was 0. 002 μg / L.[Conclusion]UPLC-MS / MS has the characteristics of high sensitivity and fast detection speed,which can be used to detect the triazophos in aquaculture water.