Dispersive liquid-liquid microextraction combined with high performance liquid chromatography-fluorescence detection
Qiuhua Wu1, Yunpeng Li, Chun Wang
1Key Laboratory of Bioinorganic Chemistry, College of Science, Agricultural University of Hebei, Baoding 071001, China.
Abstract:
A rapid and sensitive method for the determination of carbendazim (methyl benzimidazole-2-ylcarbamate, MBC) and thiabendazole (TBZ) in water and soil samples was developed by using dispersive liquid-liquid microextraction (DLLME) coupled with high performance liquid chromatography with fluorescence detection. The water samples were directly used for the DLLME extraction. For soil samples, the target analytes were first extracted by 0.1 mol L(-1) HCl. Then, the pH of the extract was adjusted to 7.0 with 2 mol L(-1) NaOH before the DLLME extraction. In the DLLME extraction method, chloroform (CHCl(3)) was used as extraction solvent and tetrahydrofuran (THF) as dispersive solvent. Under the optimum conditions, the enrichment factors for MBC and TBZ were ranged between 149 and 210, and the extraction recoveries were between 50.8 and 70.9%, respectively. The linearity of the method was obtained in the range of 5-800 ng mL(-1) for water sample analysis, and 10-1000 ng g(-1) for soil samples, respectively. The correlation coefficients (r) ranged from 0.9987 to 0.9997. The limits of detection were 0.5-1.0 ng mL(-1) for water samples, and 1.0-1.6 ng g(-1) for soil samples. The relative standard deviations (RSDs) varied from 3.5 to 6.8% (n=5). The recoveries of the method for MBC and TBZ from water samples at spiking levels of 5 and 20 ng mL(-1) were 84.0-94.0% and 86.0-92.5%, respectively. The recoveries for soil samples at spiking levels of 10 and 100 ng g(-1) varied between 82.0 and 93.4%.
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