摘要
采用气相色谱-质谱法测定大米中15种苯氧羧酸类除草剂的残留量。优化的试验条件如下:(1)提取溶剂为乙腈;(2)衍生温度为30℃;(3)衍生时间为20min;(4)净化萃取柱为Carbon TPT柱。在气相色谱分离中用PerkinElmer Elite-5MS毛细管柱为固定相,在质谱分析中采用全扫描和多反应监测模式。15种苯氧羧酸类除草剂的线性范围均为0.02~1.00mg·L^(-1),方法的检出限(3S/N)为0.001~0.006mg·kg^(-1)。以空白样品为基体进行加标回收试验,所得回收率为80.3%~103%,测定值的相对标准偏差(n=5)为4.9%~9.8%。
GC-MS was applied to the determination of residual amounts of 15 phenoxy-hydroxy-acid herbicides in rice.The optimized conditions found were as follows：（1） extraction solvent was acetonitrile;（2）derivative temperature was 30 ℃;（3） derivative time was 20 min;（4） purified extraction column was Carbon TPT column.PerkinElmer Elite-5 MS capillary column was used for GC separation.The full-scanning mode and the multiple reaction monitoring mode were adopted in MS determination.Linearity ranges of the 15 phenoxy-hydroxyacid herbicides were found between 0.02 mg·L^（-1） and 1.00 mg·L^（-1） with detection limits（3 S/N）in the range of 0.001-0.006 mg·kg^（-1）.On the base of blank sample,test for recovery was made by standard addition method and values of recovery found were in the range of 80.3%-103%,with RSD′s（n=5）in the range of 4.9%-9.8%.
出处
《理化检验（化学分册）》
CSCD
北大核心
2017年第11期1281-1285,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
贵州省科技厅联合基金项目(TN2015-9)
贵州省联合金[(2016)7374]
