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磁性羟磷灰石表面印迹聚合物在谷物样品中玉米赤霉烯酮检测前处理中的应用。

Application of magnetic hydroxyapatite surface-imprinted polymers in pretreatment for detection of zearalenone in cereal samples.

机构信息

School of Chemistry and Chemical Engineering, Henan University of Technology, Zhengzhou 450001, PR China.

School of Chemistry and Chemical Engineering, Henan University of Technology, Zhengzhou 450001, PR China; Key Laboratory of Accurate Separation and Analysis for Complex Matrix of Zhengzhou City, Zhengzhou 450001, PR China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2022 Jun 30;1201-1202:123297. doi: 10.1016/j.jchromb.2022.123297. Epub 2022 May 15.

Abstract

This study is about the combination of magnetic solid phase extraction (MSPE) and high performance liquid chromatography-fluorescence detector (HPLC-FLD) for the pre-concentration and determination of Zearalenone (ZEA) in grain sample extracts. The novel sorbent (FeO-HAP@MIPs), for selective and intelligent extraction of ZEA, was synthesized by doping FeO into the fibrous structure of hydroxyapatite nanoparticle (FeO-HAP) and subsequently wrapping with molecularly imprinted polymers. The characteristic and morphology of magnetic particles were studied by infrared spectroscopy, vibrating sample magnetometer and scanning electron microscopy. The maximum adsorption capacity was 2.89 μg/mg. It could reach the adsorption equilibrium within 5 min. The adsorption isotherm of ZEA by the FeO-HAP@MIPs were simulated. The results showed that the extraction process of ZEA with the sorbent accorded with Langmuir isotherm. The important factors affecting the extraction efficiency include elution solvent, washing solvent and the volume of them. After a serious of experiments, the optimum conditions were as follows: the volume of elution solvent was 4 mL of methanol and the washing solvent was acetonitrile-water 2:8(v/v). The calibration curve for ZEA was linear in the range of 10.00-300.00 μg/kg. The limit of detection and limit of quantitative was 2.00 μg/kg and 6.65 μg/kg, respectively. This method could provide a good reusability of 8 times and enough recoveries at three spiked levels (3, 5 and 8 ng/mL) ranging between 61.97% and 95.15% with the relative standard deviations of 1.94%∼7.44%. These results demonstrated that FeO-HAP@MIPs could be used for separation, concentration and detection of ZEA from real samples.

摘要

本研究采用磁固相萃取(MSPE)和高效液相色谱-荧光检测(HPLC-FLD)相结合的方法,对谷物样品提取物中的玉米赤霉烯酮(ZEA)进行预浓缩和测定。通过将 FeO 掺杂到羟基磷灰石纳米颗粒(FeO-HAP)的纤维结构中,并随后用分子印迹聚合物包裹,合成了用于选择性和智能提取 ZEA 的新型吸附剂(FeO-HAP@MIPs)。通过红外光谱、振动样品磁强计和扫描电子显微镜研究了磁性颗粒的特征和形态。最大吸附容量为 2.89μg/mg,可在 5min 内达到吸附平衡。对 FeO-HAP@MIPs 对 ZEA 的吸附等温线进行了模拟。结果表明,ZEA 的萃取过程符合朗缪尔等温线。影响萃取效率的重要因素包括洗脱溶剂、洗涤溶剂及其体积。经过一系列实验,优化条件如下:洗脱溶剂体积为 4mL 甲醇,洗涤溶剂为乙腈-水 2:8(v/v)。ZEA 的校准曲线在 10.00-300.00μg/kg 范围内呈线性。检测限和定量限分别为 2.00μg/kg 和 6.65μg/kg。该方法在 3 个加标水平(3、5 和 8ng/mL)下的回收率为 61.97%-95.15%,相对标准偏差为 1.94%-7.44%,可提供 8 次良好的重复使用性。结果表明,FeO-HAP@MIPs 可用于从实际样品中分离、浓缩和检测 ZEA。

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