IL/Fe_(3)O_(4)-COOH@MIL-101磁性固相萃取-高效液相色谱测定牛奶中的黄曲霉毒素  

Determination of Aflatoxins in Milk by Magnetic Solid Phase Extraction Coupled with High Performance Liquid Chromatography Using IL/Fe_(3)O_(4)-COOH@MIL-101

作　　者：陈坤 孙彬 高仕谦[1] 王学东 CHEN Kun;SUN Bin;GAO Shiqian;WANG Xuedong(School of Environmental Science and Engineering,Suzhou University of Science and Technology,Suzhou 215009)

机构地区：[1]苏州科技大学环境科学与工程学院,江苏苏州215009

出　　处：《分析科学学报》2023年第4期398-404,共7页Journal of Analytical Science

基　　金：国家自然科学基金(No.21876125,22076134);江苏省科技厅重点项目(BE2022733)。

摘　　要：基于水热合成法制备了新型材料IL/Fe_(3)O_(4)-COOH@MIL-101,通过磁性固相萃取结合高效液相色谱,建立了牛奶中4种黄曲霉毒素(AFs)的分析方法。通过傅里叶变换红外光谱(FT-IR)、扫描电镜(SEM)、透射电镜(TEM)、X射线光电子能谱(XPS)、X射线衍射(XRD)和磁滞回线(VSM)等技术分析材料的理化性质。以IL/Fe 3O 4-COOH@MIL-101作为磁性固相萃取(MSPE)的吸附剂,通过控制变量法和正交试验来优化材料的投加量、萃取时间、解吸条件和样品体积提高萃取效率,结合高效液相色谱(HPLC)-荧光检测器(FD)检测牛奶样品中4种AFs(AFB 1、AFB 2、AFG 1和AFG 2)。研究结果表明,当材料投加量为65 mg,萃取时间为17.5 min,洗脱剂为乙腈-二氯甲烷(体积比4∶1),洗脱次数为2次和样品体积为10 mL时,AFB 1和AFG 1在0.5~20μg/L范围、AFG 2在0.2~20μg/L范围及AFB 2在0.1~20μg/L范围内,目标物色谱峰面积与浓度有良好的线性关系。AFs的相关系数R^(2)均大于0.99,方法检出限为0.03~0.15μg/L,定量限为0.03~0.15μg/L。3种不同加标浓度(0.5、2、10μg/L)下,AFs加标回收率范围为76.18%~108.49%,相对标准偏差(RSD)范围为0.84%~6.47%。The novel material IL/Fe_(3)O_(4)-COOH@MIL-101 was prepared based on hydrothermal synthesis,and a method for the analysis of four aflatoxins(AFs)in milk was established by magnetic solid phase extraction combined with high performance liquid chromatography.The physicochemical properties and magnetic properties of this material were.characterized by Fourier transform infrared(FT-IR),scanning electron microscopy(SEM),transmission electron microscopy(TEM),X-ray photoelectron spectroscopy(XPS),X-ray diffraction(XRD)and Vibrating sample magnetometer(VSM).The prepared magnetic material was used as an adsorbent for magnetic solid phase extraction(MSPE)combined with high performance liquid chromatography(HPLC)-fluorescence detector(FD)to detect four AFs(AFB 1,AFB 2,AFG 1,AFG 2)in milk samples.The material dosage,extraction time,desorption conditions and sample volume were optimized by the controlled variable method and orthogonal experiment to improve the extraction efficiency.There were good linear relationships for four AFs in the range of 0.5-20μg/L for AFB 1 and AFG 1,0.2-20μg/L for AFG 2,respectively.The correlation coefficients R^(2) of AFs were all greater than 0.9977,the detection limits were 0.03-0.15μg/L,and the quantification limits were 0.03-0.15μg/L.For AFs with three different spiked concentrations(0.5,2 and 10μg/L),the spiked recoveries ranged from 76.18%-108.49%,and the relative standard deviations ranged from 0.84%-6.47%.

关 键 词：黄曲霉毒素 磁性固相萃取 离子液体 牛奶 高效液相色谱 

分 类 号：O657.72[理学—分析化学]