高级检索

    全自动加速溶剂萃取-超高效液相色谱-串联质谱法测定土壤中7种杀线虫剂的残留量

    Determination of Residues of 7 Nematocides in Soil by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry with Automatic Accelerated Solvent Extraction

    • 摘要: 通过优化提取、净化条件,提出了题示方法测定土壤样品中棉隆、噻唑膦、灭线磷、丰索磷、杀线威、丁硫环磷、除线磷等7种杀线虫剂的含量。随机采集土壤样品,风干,粉碎后过筛,分取10.0 g,加入硅藻土15.0 g,用体积比2∶1的甲醇和三氯甲烷混合溶液进行加热加压全自动萃取;萃取液过活化好的HLB固相萃取柱,用10 mL体积比1∶1的甲醇和乙腈混合溶液洗脱。洗脱液于45 ℃氮吹至近干,残留物用1 mL乙酸乙酯溶解,过0.22 μm滤膜,滤液采用超高效液相色谱-串联质谱法测定。结果显示:7种杀线虫剂的质量浓度在0.005~2.0 mg·L-1内与峰面积呈线性关系,检出限(3S/N)为4~25 μg·kg-1;按照标准加入法进行回收试验,回收率为87.2%~101%,测定值的相对标准偏差(n=6)为1.5%~3.8%;方法用于实际样品分析,检出了棉隆、噻唑膦、灭线磷、丰索磷、除线磷,检出量为14.81~124.03 μg·kg-1

       

      Abstract: By optimizing the extraction and purification conditions, the method mentioned by the title was proposed to determine 7 nematocides in soil samples, including dazomet, fosthiazate, ethoprophos, fensulfothion, oxamyl, fosthietan and dichlofenthion. Soil sample was collected randomly, dried by air, crushed and sieved. An aliquot (10.0 g) was taken, and 15.0 g of diatomaceous earth was added. The mixture was extracted automatically under heating and pressure conditions with the mixed solution of methanol and trichloromethane at volume ratio of 2∶1. The extract was passed through the activated HLB solid phase extraction column for elution by 10 mL of the mixed solution of methanol and acetonitrile at volume ratio of 1∶1. The eluent was blown to near dryness by nitrogen at 45 ℃, and the residue was dissolved in 1 mL of ethyl acetate. The solution obtained was passed through a 0.22 μm filter membrane, and the filtrate was determined by ultra-high performance liquid chromatography-tandem mass spectrometry. It was shown that linear relationships between values of the mass concentration and the peak area of the 7 nematocides were kept in the range of 0.005-2.0 mg·L-1, with detection limits (3S/N) in the range of 4-25 μg·kg-1. Test for recovery was made according to the standard addition method, giving recoveries in the range of 87.2%-101%, and RSDs (n=6) of the determined values in the range of 1.5%-3.8%. The proposed method was used for the analysis of actual samples, and dazomet, fosthiazate, ethoprophos, fensulfothion and dichlofenthion were detected with detection amounts ranged from 14.81 μg·kg-1to 124.03 μg·kg-1.

       

    /

    返回文章
    返回