摘要
以氧化琼脂糖(AG)和四甲氧基硅烷(TMOS)为前驱体,通过溶胶-凝胶法制备AG/SiO_(2)整体柱,利用酰胺化反应对整体柱进行酰胺基团修饰。通过X射线光电子能谱(XPS)、傅里叶变换红外光谱(FTIR)、N_(2)吸附-脱附和扫描电镜(SEM)等表征手段对所制备材料的结构和形貌进行分析。结果显示酰胺基团被成功修饰至整体柱,该材料具有良好的通透性及较大的比表面积。以其为固相微萃取介质对羊肉中的莱克多巴胺进行萃取富集,在优化的样品前处理条件下,采用基质添加标准曲线法,结合高效液相色谱-紫外(HPLCUV)检测,建立了羊肉中痕量莱克多巴胺的分析方法。该方法在1.94~1170 ng/g范围内线性良好,相关系数(r^(2))为0.9931,检出限(LOD)和定量下限(LOQ)分别为0.618、1.94 ng/g,3个不同加标水平下样品的平均回收率为86.6%~103%,相对标准偏差(RSD,n=5)为4.8%~7.3%。该方法具有检出限低、回收率高、样品用量少等特点,可用于羊肉中痕量莱克多巴胺的灵敏检测。
An agrose/silica(AG/SiO_(2))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),N_(2)/adsorption-desorption and scanning electron microscopy(SEM).Results indicated that amide groups were successfully modified on the surface of AG/SiO_(2) 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 solidphase 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 25μL 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 1.94-1170 ng/g with a correlation coefficient(r2)of 0.9931.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.
作者
彭传云
张少文
冯勇
吴春来
赵晓洁
宋根娣
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 471023,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2021年第8期1177-1183,共7页
Journal of Instrumental Analysis
基金
国家自然科学基金(31900005)
河南省基础前沿技术研究项目(162300410017)。
关键词
高效液相色谱
硅胶整体柱
固相微萃取
莱克多巴胺
羊肉
high performance liquid chromatography
silica monolithic column
solid-phase micro-extraction
ractopamine
mutton
