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MIL-101(Cr)填充针头式过滤器固相微萃取/高效液相色谱法检测水中雌激素
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作者单位
邓鑫雨,魏皓东,庞月红,史学丽,张 毅 1. 江南大学 食品科学与技术国家重点实验室食品学院分析食品安全研究所江苏 无锡 2141222. 石家庄市妇幼保健院河北 石家庄 050051 
基金项目:国家自然科学基金(21876066);河北医学科学研究课题计划(20212039)
中文摘要:建立了多孔金属有机骨架MIL-101(Cr)填充针头式尼龙过滤器固相微萃取结合高效液相色谱-荧光检测器对水中雌二醇(E2)、雌三醇(E3)、雌酮(E1)3种雌激素进行快速检测的方法。MIL-101(Cr)与尼龙滤膜对雌激素表现出协同吸附效果。通过对萃取材料以及新型萃取装置制备过程、吸附、洗脱过程进行优化,可对10 mL水样中3种雌激素实现4 min吸附、1 min洗脱的快速前处理。结果显示,E2和E3在0.2~500 μg/L、E1在5~500 μg/L质量浓度范围内线性良好,相关系数(r2)为0.998 2~0.999 3,检出限分别为0.05、0.06、1.50 μg/L,日内和日间相对标准偏差(RSD)分别为0.20%~3.2%(n = 6)和 5.9%~6.1%(n = 3)。水样中3种分析物的加标回收率为84.1%~108%,RSD均不大于5.5%。该方法简单方便、灵敏度高,能够用于水样中3种雌激素的快速筛查和准确定量。
中文关键词:固相微萃取(SPME)  高效液相色谱(HPLC)  金属有机骨架  MIL-101(Cr)  雌激素  尼龙过滤器
 
Determination of Estrogens in Water by High Performance Liquid Chromatography with MIL-101(Cr)Filled Syringe Filter Based Solid-phase Micro-extraction
Abstract:A novel, simple and rapid method was established for the determination of estradiol(E2), estradiol(E3) and estrone(E1) in water, based on solid-phase micro-extraction(SPME) using porous metal-organic framework MIL-101(Cr) filled syringe nylon filter combined with high performance liquid chromatography-fluorescence detector. Firstly, the MIL-101(Cr) powder material was prepared by the hydrothermal synthesis method, whose structure, crystal forms and surface properties were proved by characterization of X-ray diffraction(XRD), scanning electron microscopy(SEM), nitrogen adsorption-desorption isotherms and pore size distribution. Secondly, the integrity of the nylon membrane in the proposed SPME device was verified by simulating the solid-phase extraction process. Next, the dominant parameters affecting enrichment efficiency, including extraction speed, sample pH value, salt concentration, washing and desorption conditions were investigated. It was found that when the sample was set at pH 6.0, the salt concentration was 0, the syringe speed was 2.5 mL/min, the elution solvent was methanol, and the washing solvent was 2 mL of 10% methanol/H2O, the extraction effect for the three targets was the best. Under the optimized conditions, three target estrogens in 10 mL water sample could be adsorbed within 4 min and eluted within 1 min. This method showed good linear relationships in the range of 0.2-500 μg/L for E2 and E3, and 5-500 μg/L for E1, with their correlation coefficients(r2) of 0.998 2-0.999 3. The limits of detection for three analytes were 0.05, 0.06 and 1.50 μg/L, respectively. The relative standard deviations(RSD) for intra-day(n = 6) and inter-day(n = 3) were in the ranges of 0.20%-3.2% and 5.9%-6.1%, respectively.The recoveries for all targets in water samples at three spiked levels ranged from 84.1% to 108%, with RSDs not more than 5.5%. The developed method is simple and sensitive, and could be used for the rapid determination and accurate quantification of estrogens in water samples. In this method, MIL-101(Cr) and nylon membrane showed a synergistic adsorption effect on estrogen, providing a new strategy for multi-objective purification and extraction from complex environmental samples.
Key Words:solid-phase micro-extraction(SPME)  high performance liquid chromatography(HPLC)  metal-organic framework  MIL-101(Cr)  estrogen  nylon filter
引用本文:邓鑫雨,魏皓东,庞月红,史学丽,张 毅.MIL-101(Cr)填充针头式过滤器固相微萃取/高效液相色谱法检测水中雌激素[J].分析测试学报,2021,40(9):1271-1278.
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