分散液相微萃取-高效液相色谱法测定水样中扑虱灵和哒螨灵
HPLC Determination of Buprofezin and Pyridaben in Water Samples with Separation by Dispersion Liquid-Liquid Microextraction
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摘要: 取水样置于离心管中,与含有三氯甲烷(萃取溶剂)的乙腈(分散剂)混合溶液充分混匀,静置5 min,使水样中的扑虱灵和哒螨灵迅速富集于三氯甲烷液滴中,离心5 min,下层三氯甲烷相经减压蒸干后,加入乙腈-水(75+25)混合溶液50 μL溶解残渣,分取20 μL溶液供高效液相色谱法分析。用Symmetry C18色谱柱作固定相,流动相为乙腈-水(75+25)混合溶液,检测波长为238 nm。扑虱灵和哒螨灵的线性范围分别为2.0~100 μg·L-1和1.0~100 μg·L-1。回收率分别在81.2%~99.2%和87.3%~100.7%之间,相对标准偏差(n=5)分别在1.7%~8.3%及0.6%~9.1%之间。Abstract: Two insecticides, buprofezin (BPFZ) and pyridaben (PRDB) were separated from water sample by mixing thoroughly with a mixture containing CH3CN and CHCl3 and standing for 5 min in a centrifuge tube. After centrifuging for 5 min, the solvent CHCl3 was removed by evaporation under reduced pressure and the residue was taken up with 50 μL of mixed solvent of CH3CN and water (75+25), from which an aliquot of 20 μL was taken for HPLC analysis. Symmetry C18 column was used as stantionary phase and mixture of CH3CN and water (75+25) as mobile phase. UV detection at 238 nm was adopted in the determination. Linearity ranges were found between 2.0-100 μg·L-1 (for BPFZ) and 1.0-100 μg·L-1 (for PRDB). Values of recovery and RSD′s (n=5) found were in the ranges of 81.2%-99.2%, 87.3%-100.7%, and 1.7%-8.3%, 0.6%-9.1% respectively.
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