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 shu

Selective Extraction of Lead from Water and Food Samples by Dicyclohexy-18-crown-6-Dual Cloud Point Extraction Method

MAO Yan-Li ¹ ,
HAN Juan ^2,, ,
CUI Wan-Jing ³ ,
WANG Yun ³ ,
TANG Xu ³ ,
XIA Jin-Chen ³ ,
LIU Ying-Ying ³

1.
¹ School of Municipal and Environmental Engineering, Henan University of Urban Construction, Pingdingshan 467036, China;
2.
² School of Food and Biological Engineering, Jiangsu University, Zhenjiang 212013, China;
3.
³ School of Chemistry and Chemical Engineering, Jiangsu University, Zhenjiang 212013, China

Corresponding author: HAN Juan,
Received Date: 7 August 2015
Available Online: 13 September 2015
Fund Project: 本文系国家自然科学基金资助项目(Nos.31470434,21406090) (Nos.31470434,21406090)江苏出入境检验检疫局科技计划项目(No.2015KJ27) (No.2015KJ27)

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.
- Dicyclohexyl-18-crown-6,
- Dual cloud point extraction,
- Thermoseparating triblock copolymer L64,
- Lead
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沈阳化工大学材料科学与工程学院沈阳 110142

Selective Extraction of Lead from Water and Food Samples by Dicyclohexy-18-crown-6-Dual Cloud Point Extraction Method

南开大学师唯/华北电力大学（保定）刘景维：二维配位聚合物中有序的亲锂冠醚位点用于无枝晶锂沉积

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