CN106749903B - 一种双亲性乙草胺磁性分子印迹聚合物及其制备方法和应用 - Google Patents
一种双亲性乙草胺磁性分子印迹聚合物及其制备方法和应用 Download PDFInfo
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Abstract
本发明提供一种双亲性乙草胺磁性分子印迹聚合物及其制备方法和应用。以葡萄糖为结构单元,合成修饰有印迹作用位点的亲水性烯基苷型功能单体。采用“亲水‑疏水”双功能单体分子印迹技术,制备双亲性磁性分子印迹聚合物。制备的分子印迹聚合物特异选择性高、具有双亲性、在水介质中具有较好的吸附性能,能够用于农产品中乙草胺含量测定样品前处理,继而经液相色谱系统分析检测及定量分析,建立了用于复杂样品前处理的萃取体系。步骤简单、操作方便、实用性强。
Description
技术领域
本发明属于分离分析技术领域,具体涉及是一种用于检测乙草胺的双亲性磁性分子印迹聚合物的制备方法和应用。
背景技术
乙草胺除草剂是目前生产中应用较为广泛的一类芽前除草剂,除草效果较好,但具有较高的残留毒性,美国环境保护局已将乙草胺定为B-2类致癌物。由于乙草胺除草剂的水溶性较高且易于淋溶,而土壤吸附常数又相对较低,所以施到农田的酰胺类除草剂容易通过渗透转移到浅层地下水或随雨水径流进入地表水。欧盟规定农产品中乙草胺最大残留量不超过0.02mg/Kg,因此对乙草胺除草剂的分析检测极为重要。目前乙草胺除草剂的检测方法主要有色谱法、色谱-质谱联用法、酶联免疫吸附分析法,但这些方法的前处理主要采用传统的固相萃取或液液萃取,特异性差,容易导致大量基质共萃取而影响目标分析物的测定。因此建立一种快速、高效的酰胺类除草剂分析方法具有重要意义。
磁性分子印迹固相萃取是近年快速发展起来的样品前处理技术,广泛应用于食品检测、生物分离、环境检测等领域。磁性分子印迹聚合物材料是融合磁性粒子特性与分子印迹技术的一种新型分离材料.它同时具有磁性粒子的磁响应性和MIP对目标分子的特定识别力和亲和力。利用磁性粒子特性,在外加磁场作用下使聚合物达到快速富集,较传统固相萃取技术省去了复杂的离心过程,提高了聚合物的可控性。因此,将磁性分子印迹聚合物应用于固相萃取已得到学术界广泛关注。但是利用双亲性磁性分子印迹技术,选择性检测农产品中乙草胺含量的技术未见报道。
发明内容
为了克服上述不足,本发明以葡萄糖为结构单元,合成修饰有印迹作用位点的亲水性烯基苷型功能单体。采用“亲水-疏水”双功能单体分子印迹技术,制备双亲性磁性分子印迹聚合物。制备的分子印迹聚合物特异选择性高、具有双亲性、在亲水介质中具有较好的吸附性能,能够用于农产品中乙草胺含量测定样品前处理,继而经液相色谱系统分析检测及定量分析,建立了用于复杂样品前处理的萃取体系。
为了实现上述目的,本发明采用如下技术方案:
一种用于检测乙草胺的双亲性磁性印迹聚合物的制备方法,以乙草胺为模板,以Fe3O4为磁性载体,与疏水性功能单体、亲水性功能单体混合均匀后,在交联剂、引发剂、致孔剂存在条件下,聚合而成;
所述亲水性功能单体的结构通式为:
本发明中“亲水-疏水”双功能单体的构建有效提高了乙草胺分离效率,使样品前处理在3分钟之内完成,远远优于现有技术的样品前处理时间30分钟。
优选的,所述四氧化三铁、模板乙草胺、疏水性功能单体、亲水性功能单体、交联剂、引发剂、致孔剂的质量比为1~3:1~3:2~6:1~3:15~30:0.05~0.10:20~70。
优选的,所述疏水性功能单体为4-乙烯基吡啶,乙烯基苯,1-乙烯基咪唑。
优选的,所述交联剂为N,N-亚甲基二丙烯酰胺、乙二醇二甲基丙烯酸酯或二乙烯基苯。
优选的,所述引发剂为偶氮二异戊腈或偶氮二异丁腈。
优选的,所述致孔剂为去离子水。
优选的,所述聚合条件为40~60℃条件下聚合18~24小时。
优选的,所述原料在聚合反应之前,还进行超声处理和惰性气体保护。
本发明的优选实施例中,对双亲性乙草胺磁性印迹聚合物的制备方法进行了优化,具体包括以下步骤:
(1)将四氧化三铁、模板乙草胺、疏水性功能单体、亲水性功能单体、交联剂、引发剂、致孔剂按质量比为1~3:1~3:2~6:1~3:15~30:0.05~0.10:20~70加入到反应釜中充分混合;
(2)将步骤1)中的混合溶剂,超声10-15分钟,然后充氮气10-20分钟除氧;
(3)密封后于40~60℃条件下聚合18~24小时,得到带模板分子的聚合物;
(4)将步骤3)得到的聚合物磁性分离收集、筛分后用酸洗液洗脱除去模板分子;
(5)将除去模板分子的聚合物真空下50~65℃烘干干燥,即得到双亲性乙草胺磁性印迹聚合物;
其中,步骤(1)中,所述疏水性功能单体为4-乙烯基吡啶,乙烯基苯,1-乙烯基咪唑;亲水性功能单体为烯基苷型功能单体;交联剂为N,N-亚甲基二丙烯酰胺、乙二醇二甲基丙烯酸酯或二乙烯基苯;致孔剂为乙醇;引发剂为偶氮二异戊腈或偶氮二异丁腈。优选上述步骤4)得到的聚合物研磨过150~200目筛,除去模板分子用酸洗液为体积分数10%~20%的乙酸乙醇溶液。
本发明还提供了任一上述的方法制备的检测乙草胺的双亲性磁性印迹聚合物。
本发明还提供了上述双亲性磁性印迹聚合物在农产品乙草胺富集、分离、检测中的应用。
本发明还提供了上述用于检测乙草胺含量的双亲性磁性分子印迹聚合物在农产品乙草胺检测中的应用,其特征在于,包括如下步骤:以上述的分子印迹聚合物分散于农产品提取液中,震荡吸附1分钟,30秒内磁性分离收集聚合物,再用甲醇/乙酸混合物(95:5,v/v)脱附1分钟,脱附液进行液相检测。
其中,农产品包括小麦、大豆、花生、玉米、大米、小米;
农产品提取液为:10克农产品用100克乙醇回流提取2小时,过滤出去不溶物,既得;
印迹聚合物与农产品提取液的用量(重量)比为:1:1000~1:5000;
分子印迹聚合物的再生重复利用:将分子印迹聚合物用95%乙醇洗脱后即可再生用于下一次纯化富集用。
本发明的有益效果
(1)本发明以葡萄糖为结构单元,合成修饰有印迹作用位点的亲水性烯基苷型功能单体。采用“亲水-疏水”双功能单体分子印迹技术,制备双亲性磁性分子印迹聚合物。制备的分子印迹聚合物特异选择性高、具有双亲性、在亲水介质中具有较好的吸附性能,能够用于农产品中乙草胺含量测定样品前处理,继而经液相色谱系统分析检测及定量分析,建立了用于复杂样品前处理的萃取体系。
(2)本发明建立的样品前处理方法耗时短,3分钟之内完成,简便快速。
(3)本发明操作过程均以乙醇为主要溶剂,避免使用毒性较高的有机溶剂,绿色环保。
具体实施方式
以下通过实施例对本发明特征及其它相关特征作进一步详细说明,以便于同行业技术人员的理解:
实施例1
双亲性乙草胺磁性分子印迹聚合物的制备:
(1)备料
各原料组分按如下用量配比配料:四氧化三铁0.91克,模板乙草胺0.91g,烯基苷型功能单体(结构式如式Ⅰ所示)0.91g,二乙烯基苯1.98克,交联剂N,N-亚甲基二丙烯酰胺16.17g,引发剂偶氮二异丁腈0.08g,制孔剂乙醇55.31g;
(2)制备带有模板分子的分子印迹聚合物
将上述备好的反应物加入到反应釜中混合均匀,超声脱气15min,然后充氮除氧15分钟,密封后于60℃恒温油浴聚合24小时,得到带有模板分子的聚合物;
(3)制备脱去模板分子的分子印迹聚合物
将上述制备的聚合物碾磨过200目筛,即得到带有模板分子的聚合物颗粒,用乙酸体积分数为10%的乙醇溶液洗脱,于60℃真空干燥后,得到分子印迹聚合物17.1g。
双亲性乙草胺磁性分子印迹聚合物在检测农产品乙草胺中的应用:
称取小麦10g粉碎,加入100克乙醇加热回流提取2小时,过滤,收集滤液。称取0.1克印迹聚合物,分散到小麦提取液中,震荡吸附1分钟,30秒磁性分离收集聚合物,再用甲醇/乙酸混合物(95:5,v/v)脱附1分钟,脱附液进行液相检测。结果表明,由本发明建立的方法得到的小麦中乙草胺含量为0.2μg/Kg。
实施例2
双亲性乙草胺磁性分子印迹聚合物的制备:
(1)备料
各原料组分按如下用量配比配料:四氧化三铁0.91克,模板乙草胺0.91g,烯基苷型功能单体(结构式如式Ⅰ所示)0.91g,4-乙烯基吡啶1.98克,交联剂乙二醇二甲基丙烯酸酯16.17g,引发剂偶氮二异戊腈0.08g,制孔剂乙醇55.31g;(2)制备带有模板分子的分子印迹聚合物
将上述备好的反应物加入到反应釜中混合均匀,超声脱气15min,然后充氮除氧15分钟,密封后于40℃恒温油浴聚合18小时,得到带有模板分子的聚合物;
(3)制备脱去模板分子的分子印迹聚合物
将上述制备的聚合物碾磨过200目筛,即得到带有模板分子的聚合物颗粒,用乙酸体积分数为10%的乙醇溶液洗脱,于60℃真空干燥后,得到分子印迹聚合物17.1g。
双亲性乙草胺磁性分子印迹聚合物在检测农产品乙草胺中的应用:
称取小麦10g粉碎,加入100克乙醇加热回流提取2小时,过滤,收集滤液。称取0.1克印迹聚合物,分散到小麦提取液中,震荡吸附1分钟,30秒磁性分离收集聚合物,再用甲醇/乙酸混合物(95:5,v/v)脱附1分钟,脱附液进行液相检测。结果表明,由本发明建立的方法得到的小麦中乙草胺含量为0.2μg/Kg。
实施例3
双亲性乙草胺磁性分子印迹聚合物的制备:
(1)备料
各原料组分按如下用量配比配料:四氧化三铁0.91克,模板乙草胺0.91g,烯基苷型功能单体(结构式如式Ⅰ所示)0.91g,乙烯基苯1.98克,交联剂乙二醇二甲基丙烯酸酯16.17g,引发剂偶氮二异戊腈0.08g,制孔剂乙醇55.31g;
(2)制备带有模板分子的分子印迹聚合物
将上述备好的反应物加入到反应釜中混合均匀,超声脱气15min,然后充氮除氧15分钟,密封后于50℃恒温油浴聚合20小时,得到带有模板分子的聚合物;
(3)制备脱去模板分子的分子印迹聚合物
将上述制备的聚合物碾磨过200目筛,即得到带有模板分子的聚合物颗粒,用乙酸体积分数为10%的乙醇溶液洗脱,于60℃真空干燥后,得到分子印迹聚合物17.1g。
双亲性乙草胺磁性分子印迹聚合物在检测农产品乙草胺中的应用:
称取小麦10g粉碎,加入100克乙醇加热回流提取2小时,过滤,收集滤液。称取0.1克印迹聚合物,分散到小麦提取液中,震荡吸附1分钟,30秒磁性分离收集聚合物,再用甲醇/乙酸混合物(95:5,v/v)脱附1分钟,脱附液进行液相检测。结果表明,由本发明建立的方法得到的小麦中乙草胺含量为0.2μg/Kg。
实施例4
双亲性乙草胺磁性分子印迹聚合物的制备:
(1)备料
各原料组分按如下用量配比配料:四氧化三铁0.91克,模板乙草胺0.91g,烯基苷型功能单体(结构式如式Ⅰ所示)0.91g,1-乙烯基咪唑1.98克,交联剂二乙烯基苯16.17g,引发剂偶氮二异丁腈0.08g,制孔剂乙醇55.31g;
(2)制备带有模板分子的分子印迹聚合物
将上述备好的反应物加入到反应釜中混合均匀,超声脱气15min,然后充氮除氧15分钟,密封后于55℃恒温油浴聚合22小时,得到带有模板分子的聚合物;
(3)制备脱去模板分子的分子印迹聚合物
将上述制备的聚合物碾磨过200目筛,即得到带有模板分子的聚合物颗粒,用乙酸体积分数为10%的乙醇溶液洗脱,于60℃真空干燥后,得到分子印迹聚合物17.1g。
双亲性乙草胺磁性分子印迹聚合物在检测农产品乙草胺中的应用:
称取小麦10g粉碎,加入100克乙醇加热回流提取2小时,过滤,收集滤液。称取0.1克印迹聚合物,分散到小麦提取液中,震荡吸附1分钟,30秒磁性分离收集聚合物,再用甲醇/乙酸混合物(95:5,v/v)脱附1分钟,脱附液进行液相检测。结果表明,由本发明建立的方法得到的小麦中乙草胺含量为0.2μg/Kg。
最后应该说明的是,以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述实施例所记载的技术方案进行修改,或者对其中部分进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。上述虽然对本发明的具体实施方式进行了描述,但并非对本发明保护范围的限制,所属领域技术人员应该明白,在本发明的技术方案的基础上,本领域技术人员不需要付出创造性劳动即可做出的各种修改或变形仍在本发明的保护范围以内。
Claims (10)
1.一种用于检测乙草胺的双亲性磁性印迹聚合物的制备方法,其特征在于,以乙草胺为模板,以Fe3O4为磁性载体,与疏水性功能单体、亲水性功能单体混合均匀后,在交联剂、引发剂、致孔剂存在条件下,聚合而成;
所述亲水性功能单体的结构通式为:
2.如权利要求1所述的方法,其特征在于,所述四氧化三铁、模板乙草胺、疏水性功能单体、亲水性功能单体、交联剂、引发剂、致孔剂的质量比为1~3:1~3:2~6:1~3:15~30:0.05~0.10:20~70。
3.如权利要求1所述的方法,其特征在于,所述疏水性功能单体为4-乙烯基吡啶,乙烯基苯,1-乙烯基咪唑。
4.如权利要求1所述的方法,其特征在于,所述交联剂为N,N-亚甲基二丙烯酰胺、乙二醇二甲基丙烯酸酯或二乙烯基苯。
5.如权利要求1所述的方法,其特征在于,所述引发剂为偶氮二异戊腈或偶氮二异丁腈。
6.如权利要求1所述的方法,其特征在于,所述致孔剂为乙醇。
7.如权利要求1所述的方法,其特征在于,所述聚合条件为40~60℃条件下聚合18~24小时。
8.如权利要求1所述的方法,其特征在于,原料在聚合反应之前,还进行超声处理和惰性气体保护。
9.权利要求1-8任一项所述的方法制备的检测乙草胺的双亲性磁性印迹聚合物。
10.权利要求9所述的双亲性磁性印迹聚合物在农产品乙草胺富集、分离、检测中的应用。
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