Novel surface molecularly imprinted sol-gel polymer applied to the online solid phase extraction of methyl-3-quinoxaline-2-carboxylic acid and quinoxaline-2-carboxylic acid from pork muscle |
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Authors: | Duan Zhen-Juan Fan Li-Peng Fang Guo-Zhen Yi Jiang-Hua Wang Shuo |
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Institution: | (1) Key Laboratory of Food Nutrition and Safety, Ministry of Education of China, Tianjin University of Science and Technology, Tianjin, 300457, China; |
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Abstract: | A new molecularly imprinted polymer (MIP), selective for major metabolites of quinoxaline-1,4-dioxides was firstly prepared
by combining surface molecular imprinting technique with the sol–gel process. Methyl-3-quinoxaline-2-carboxylic acid (MQCA)
was used as template, 3-aminopropyltriethoxysilane as functional monomer, and tetraethoxysilicane as cross-linker. The MIP
was characterized by Fourier transform infrared and evaluated through static adsorption experiments. The results indicated
that MIP had high adsorption capacity, fast binding kinetics for MQCA, and the polymer showed a high degree of cross-reactivity
for quinoxaline-2-carboxylic acid (QCA). The MIP was then applied as a selective sorbent in an online solid phase extraction
(SPE) coupled with high-performance liquid chromatography (HPLC). For a 50-mL sample solution, enrichment factors of 1,349
and 1,046 for QCA and MQCA, respectively, and limits of detection (S/N = 3) of 0.8 and 2 ng L−1 for QCA and MQCA, respectively, were obtained (corresponding to 0.02 and 0.04 ng g−1 in solid samples for final 100 mL of sample solutions of 5 g of pork). The sample preparation protocol was simplified and
only included one step extraction with acetonitrile (MeCN) after the release of target analytes through acidic hydrolysis
without further sample cleanup. The new MIP-SPE-HPLC method was successfully applied to the quantification of trace QCA and
MQCA in pork muscle with good recoveries ranging from 67% to 80% and RSD below 8%. |
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