实时直接分析-串联质谱法快速测定环境水体中涕灭威及其代谢物

Rapid Determination of Aldicarb and Its Metabolites in Water Environment by Real-Time Direct Analysis-Tandem Mass Spectrometry

  • 摘要: 建立了实时直接分析-串联质谱法快速测定环境水体中涕灭威及其代谢物,通过优化实时直接分析离子源的离子化气体温度、采样速度、外置真空泵真空度、点样量及点样方式、点样位置等参数,使用三重四极杆质谱正离子模式直接进样分析。结果表明,最佳检测条件是离子化气体温度300 ℃、采样速度0.6 mm/s、外置真空泵真空度-70 kPa、点样量10 μL、点样位置1~5 mm。在该条件下,涕灭威及其代谢物分别在0.5~10 μg/L和0.1~10 μg/L浓度范围内的线性关系良好,线性相关系数为0.995 6~0.998 9。本方法的检出限为0.1~0.7 μg/L,添加回收率为94%~102%。该方法简单、快捷,可实现环境水体中涕灭威及其代谢物的实时直接和高通量检测。

     

    Abstract: Aldicarb, aldicarb sulfoxide (aldicarb) and aldicarb sulfoxide (aldicarb) are carbamate insecticide and acaricide, which are widely used in the growth of crops. Aldicarb and its metabolites will create pollution for aquatic environment during the spraying process, and enter the human body directly or indirectly. At present, the detection standard of aldicarb and its metabolites in water environment has the problems of complicated sample pretreatment process and long time consuming in instrument detection, it is difficult to meet the demand of increasing sample size. Therefore, it is of great significance to establish a rapid detection method for alidcarb and its metabolites in different water environment. In this study, the parameters of ionization gas temperature, sampling speed, vacuum degree of external vacuum pump, point sample quantity, point sample mode, point sample position were optimized. There were two problems in the determination of alidcarb and its metabolites in water environment by real-time direct analysis ion source. Firstly, the real-time direct analysis ion source is an open ion source, after the analyte was ionized in the open environment, the parallelism between the samples was poor because of the difference in the amount of analyte entering the mass spectrometry. The difference of ionization efficiency between the parallel samples due to the different positions of the target compound in TIP leads to the poor parallelism. Secondly, if the solvent of the water sample cannot completely volatilize after sampling, the water solvent will consume too much energy in the process of ionization, the target material cannot be sufficiently ionized because it cannot distribute enough energy, which affects the detection sensitivity. A rapid method for the determination of aldicarb and its metabolites in water environment was established. The results showed that the best detection condition was when the temperature of ionized gas was 300 ℃, the sampling speed was 0.6 mm/s, the vacuum degree of external vacuum pump was -70 kPa, the sample amount was 10 L and the sample position was 1.5 mm. Under the optimized conditions, 0.5-10 g/L for aldicarb and 0.1-10 g/L for its metabolites had good linear relationship with the correlation coefficient of 0.995 6-0.998 9. The detection limit was 0.1-0.5 g/L and the recovery was 94%-109%. This method is simple and rapid, which can be used to detect aldicarb and its metabolites in water environment in real-time and high-throughput.

     

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