摘要
提出了全自动固相萃取-高效液相色谱-串联质谱法测定耕地周边地表水中乙嘧酚、嘧菌环胺、氟嘧菌胺、嘧菌腙、嘧霉胺、氯苯嘧啶醇等6种嘧啶类杀菌剂残留量的方法。分取预处理后的地表水样品500 mL,调节酸度至pH(7.00±0.05),以18 mL·min^(-1)流量过活化好的HLB固相萃取柱(500 mg/12 mL),用体积比1:1的甲醇-乙腈混合溶液洗脱,收集洗脱液,于45℃氮吹至近干,加入甲醇1 mL复溶,涡旋混匀后上机检测。结果表明:6种嘧啶类杀菌剂的质量浓度均在0.01~5.00μg·mL^(-1)内与对应的质谱响应值呈线性关系,检出限(3S/N)为0.007~0.033μg·L^(-1);按照标准加入法进行回收试验,回收率为84.8%~102%,测定值的相对标准偏差(RSD,n=5)为1.5%~3.6%,重复性RSD(n=6)为1.9%~2.9%。
A method for the determination of residues of 6 pyrimidine fungicides,including ethirimol,cyprodinil,diflumetorim,ferimzone,pyrimethanil and fenarimol in surface water around cultivated land by high performance liquid chromatography-tandem mass spectrometry with automatic solid phase extraction was proposed.An aliquot(500 mL)of surface water sample after pretreatment was taken,and its acidity was adjusted to pH(7.00±0.05).Then the above water sample was passed through the activated HLB solid phase extraction column(500 mg/12 mL)at a flow rate of 18 mL·min^(-1),and eluted with the mixed solution of methanol and acetonitrile at volume ratio of 1:1.The eluent was collected,and blown to nearly dryness by nitrogen at 45℃,and 1 mL of methanol was added for redissolution.The mixed solution was tested by the instrument after mixing well by vortex.It was shown that linear relationships between the mass concentrations and their corresponding MS response values of 6 pyrimidine fungicides were kept in the same range of 0.01-5.00μg·mL^(-1),with detection limits(3S/N)in the range of 0.007-0.033μg·L^(-1).Test for recovery was made according to the standard addition method,giving results in the range of 84.8%-102%,with RSDs(n=5)of the determined values in the range of 1.5%-3.6%,and RSDs(n=6)of the reproducibility in the range of 1.9%-2.9%.
作者
倪洁
孙志洪
毛娜
NI Jie;SUN Zhihong;MAO Na(Hengshui Ecological Environment Monitoring Center of Hebei Province,Hengshui 053000,China;Cangzhou Ecological Environment Monitoring Center of Hebei Province,Cangzhou 061000,China;Cangzhou Academy of Ecological and Environmental Protection,Cangzhou 061000,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2024年第1期22-26,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
关键词
全自动固相萃取
高效液相色谱-串联质谱法
耕地周边地表水
嘧啶类杀菌剂
automatic solid phase extraction
high performance liquid chromatography-tandem mass spectrometry
surface water around cultivated land
pyrimidine fungicide
