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| Preparation of Amide Modified Silica Hy? brid Monolithic Column and Its Application in Ractopamine Determination |
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| DOI： |
| KeyWord:high performance liquid chromatography ?silica monolithic column ?solid-phase micro-extraction ?ractopamine ?mutton |
| Author | Institution |
| PENG Chuan-yun，ZHANG Shao-wen，FENG Yong， WU Chun-lai，ZHAO Xiao-jie，SONG Gen-di |
School of Environmental Engineering and Chemistry，Luoyang Institute of Science and Technology， Luoyang ，China |
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| Abstract: |
| An agrose/silica（AG/SiO2） monolithic column was prepared via sol－gel reaction with oxide agrose（AG） and tetramethoxysilane（TMOS） as precursors， and then amide groups were modified through amidation reaction. The structure and morphology of the prepared monolithic column were investigated by X-ray photoelectron spectroscopy（XPS）， Fourier transform infrared spectroscopy（FTIR）， N2/adsorption－desorption and scanning electron microscopy（SEM）. Results indicated that amide groups were successfully modified on the surface of AG/SiO2 monolithic column. The monolith possessed satisfactory permeability and larger specific surface area which could contribute to better extraction and enrichment efficiency. Thereafter， the monolith was used as solid-phase micro-extraction pattern for extraction and enrichment of ractopamine in mutton samples. The pretreatment conditions of real samples were optimized thoroughly， including extraction solvent， pH value， extraction rate， elution rate and elution volume. As a result， the optimized conditions such as an extraction solvent of acetonitrile－water（7∶3）， a pH value of 5.6， an extraction rate of 0.05 mL/min， an elution rate of 0.03 mL/min and an elution volume of 25 μL were used for cleaning up ractopamine from mutton samples. Under the optimized sample pretreatment conditions， coupled with common high performance liquid chromatography with ultraviolet detection（HPLC－UV）， a method for determination of ractopamine was established by using a matrix addition standard curve. The linear range of the method was 1.94－1 170 ng/g with a correlation coefficient（r2） of 0.993 1. The limit of detection（LOD，?S/N?= 3） was 0.618 ng/g， while the limit of quantitation（LOQ，?S/N?= 10） was 1.94 ng/g. The recoveries at three spiked levels ranged from 86.6% to 103%， with relative standard deviations（RSD） of 4.8%－7.3% by repeating the same experiment for 5 times. The established method was applicable for detection of trace residue of ractopamine in real mutton samples with the advantages of sensitivity， efficiency， reliability， high recovery and low usage of samples. |
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