Citation:
MAO Yan-Li, HAN Juan, CUI Wan-Jing, WANG Yun, TANG Xu, XIA Jin-Chen, LIU Ying-Ying. Selective Extraction of Lead from Water and Food Samples by Dicyclohexy-18-crown-6-Dual Cloud Point Extraction Method[J]. Chinese Journal of Analytical Chemistry,
;2016, 44(1): 131-137.
doi:
10.11895/j.issn.0253-3820.150630
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A new extraction method, dicyclohexyl-18-crown-6 (DCH18C6)-dual cloud point extraction method (DCH18C6-DCPE), was developed for extraction and determination of Pb in environmental water and food samples. The DCH18C6-DCPE method included two cloud point extraction (CPE) steps. At the first CPE procedure, DCH18C6 was used as selective chelating agent of Pb2+, and the formed hydrophobic complex (Pb-DCH18C6) was entrapped in a thermoseparating triblock copolymer (L64) rich phase. At the second CPE stage, the L64-rich phase was treated with a certain amount of Ethylene Diamine Tetraacetic Acid (EDTA) solution, and Pb2+ was back extracted into the aqueous phase for analysis due to its stronger combining capacity with EDTA. The single factor experiment and response surface methodology design were used to obtain the optimal condition, namely 2.06% L64 (m/m), 8.13% K2HPO4(m/m), 207.23 μg/mL DCH18C6, 70℃ of extraction temperature, and 10 min of extraction time. Under the optimized conditions, the calibration curve was linear in the range of 0.05-0.3 μg/mL (R2=0.998), the extraction efficiency of Pb was 98.8%, and the limit of detection (LOD) was 2.8 μg/L. Besides, the precisions of inter-day RSD<4.6% and intra-day RSD<6.8% were obtained. Moreover, the proposed method was successfully applied to the determination of Pb2+ in water and food samples with the recoveries of 97.3%-102.2% and a relative standard deviation (RSD) lower than 3.7%. The results indicated that the proposed method was effective for the determination of Pb2+ in real samples.
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