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    李丹娜, 王建山. 复合离子液体修饰硅胶嵌套海绵材料固相萃取-超高效液相色谱法测定环境水中黄曲霉毒素B1的含量[J]. 理化检验-化学分册, 2024, 60(8): 758-763. DOI: 10.11973/lhjy-hx230305
    引用本文: 李丹娜, 王建山. 复合离子液体修饰硅胶嵌套海绵材料固相萃取-超高效液相色谱法测定环境水中黄曲霉毒素B1的含量[J]. 理化检验-化学分册, 2024, 60(8): 758-763. DOI: 10.11973/lhjy-hx230305
    LI Danna, WANG Jianshan. Determination of Aflatoxin B1 in Environmental Water by Ultra-High Performance Liquid Chromatography after Solid Phase Extraction with Composite Ionic Liquid Modified Silica Gel Nested Sponge Material[J]. PHYSICAL TESTING AND CHEMICAL ANALYSIS PART B:CHEMICAL ANALYSIS, 2024, 60(8): 758-763. DOI: 10.11973/lhjy-hx230305
    Citation: LI Danna, WANG Jianshan. Determination of Aflatoxin B1 in Environmental Water by Ultra-High Performance Liquid Chromatography after Solid Phase Extraction with Composite Ionic Liquid Modified Silica Gel Nested Sponge Material[J]. PHYSICAL TESTING AND CHEMICAL ANALYSIS PART B:CHEMICAL ANALYSIS, 2024, 60(8): 758-763. DOI: 10.11973/lhjy-hx230305

    复合离子液体修饰硅胶嵌套海绵材料固相萃取-超高效液相色谱法测定环境水中黄曲霉毒素B1的含量

    Determination of Aflatoxin B1 in Environmental Water by Ultra-High Performance Liquid Chromatography after Solid Phase Extraction with Composite Ionic Liquid Modified Silica Gel Nested Sponge Material

    • 摘要: 将功能化离子液体制备的复合离子液体用于修饰硅胶嵌套海绵材料,采用场发射扫描电子显微镜和傅里叶变换红外光谱仪对该复合材料的性能进行表征。将复合材料装填于一次性使用无菌注射器制备固相萃取柱,并考察了其吸附容量。水样经除杂、过滤后,取续滤液1.5 L,以3 mL·min−1流量过上述制备好的固相萃取柱,用5 mL水淋洗,3 mL体积比1∶5的丙酮-2 mol·L−1盐酸溶液的混合液洗脱,收集洗脱液,过0.45 μm有机系滤膜,滤液按照色谱条件测定。以Eclipse Plus C18色谱柱作固定相,体积比68∶32的水和体积比1∶1的乙腈-甲醇溶液的混合溶液作流动相进行等度洗脱,荧光检测器测定黄曲霉毒素B1(AFB1)的含量。结果显示:合成的复合材料中具有六圆环网状结构的海绵骨架和离子液体修饰的硅胶大颗粒物质相互嵌套,形成了类似于钢筋混凝土的结构,兼具离子液体的良好选择性和海绵的机械柔性;制备的固相萃取柱对AFB1的吸附容量为26.48 mg·g−1,显著高于文献报道的用于吸附黄曲霉毒素吸附材料的(0.460~4.289 mg·g−1);AFB1的质量浓度在0.1~40 μg·L−1内和峰面积呈线性关系,测定下限为0.2 ng·L−1;按照标准加入法进行回收试验,回收率为75.2%~95.3%,测定值的相对标准偏差(n=6)为6.9%~8.4%。

       

      Abstract: Composite ionic liquid prepared by functionalization of ionic liquids was used to modify silica gel nested sponge materials, and properties of the composite material were characterized by field emission scanning electron microscopy and Fourier transform infrared spectrometer. Composite materials were loaded into a disposable sterile syringes to prepare solid phase extraction column, adsorption capacity of which was investigated. After impurity removal and filtration of the water sample, 1.5 L of the continuation filtrate was taken and passed through the prepared solid phase extraction column at flow rate of 3 mL·min−1. The column was rinsed by 5 mL of water and eluted by 3 mL of mixed solution of acetone and 2 mol·L−1 hydrochloric acid solution at volume ratio of 1∶5. The eluate was collected and passed through a 0.45 μm organic filter membrane, and the filtrate was analyzed according to chromatographic conditions. Eclipse Plus C18 chromatographic column was used as the stationary phase, and aflatoxin B1 (AFB1) was separated by isocratic elution with the mixed solution of water and acetonitrile-methanol solution (volume ratio of 1∶1) at volume ratio of 68∶32 as the mobile phase, and detected by the fluorescence detector. It was shown that the sponge skeleton with the six ring network structure and the silica gel large particle material modified with ionic liquids in the synthesized composite material nested together, forming a structure similar to reinforced concrete, which combined the good selectivity of ionic liquids and the mechanical flexibility of sponges. The prepared solid phase extraction column had an adsorption capacity of 26.48 mg·g−1 for AFB1, significantly higher than the aflatoxin adsorption capacity (0.460-4.289 mg·g−1) of adsorption materials reported in literatures. Linear relationship between values of the mass concentration and the peak area of AFB1 was kept in the range of 0.1-40 μg·L−1, and the lower limit of determination was 0.2 ng·L−1. Test for recovery was made according to the standard addition method, giving recoveries in the range of 75.2%-95.3%, and RSDs (n=6) of the determined values ranged from 6.9% to 8.4%.

       

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