CN104764722A - 一种光聚合法制备亲水性荧光纳米球及其在2,4,6-三硝基甲苯爆炸物检测中的应用 - Google Patents
一种光聚合法制备亲水性荧光纳米球及其在2,4,6-三硝基甲苯爆炸物检测中的应用 Download PDFInfo
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Abstract
本发明公开了一种亲水性荧光纳米球的制备方法及其在2,4,6-三硝基甲苯爆炸物检测中的应用。本发明采用光激发原位聚合法,将油相量子点聚合为亲水性荧光纳米球,通过调控烯丙基硫醇单体的加入量,可以得到粒径尺寸在50-100nm间调变的纳米球。修饰在纳米球表面的氨基可与2,4,6-三硝基甲苯在强碱性条件下特异性结合,并发生电子转移,使其在350-600nm间有一宽吸收峰,在342nm近红外光的激发下,与硫化锌掺锰量子点纳米颗粒的591nm处的发射峰发生重叠,产生有效的荧光淬灭,可以通过检测荧光强度,达到定性定量检测2,4,6-三硝基甲苯的目的。与传统的检测方法比较,该方法操作简单,背景干扰小,信号强,成本低,且具有检测限低,快速准确,灵敏度高的特点。
Description
技术领域
本发明属于硝基爆炸物传感和检测技术领域,特别涉及一种原位光聚合法制备亲水性荧光纳米球及其在2,4,6-三硝基甲苯爆炸物检测中的应用。
技术背景
随着社会的发展,人们越来越重视国土安全,人类健康和绿色环境,炸药残留物和爆炸类似物的检测,吸引了科学的关注,并成为应对恐怖主义威胁,土壤和地下水污染的重要国际问题,爆炸物及其类似物的快速、灵敏、选择性分析是分析化学界与社会最为关注的领域之一。根据化学性质分类,炸药可分为硝基芳烃,硝酸酯,重氮盐化合物和过氧化物。其中,2,4,6-三硝基甲苯作为一种重要的爆炸物被广泛运用于军工生产和民用爆破中,由于其是一种高毒性的致癌化合物,因此在生产和使用过程中,很容易渗入土壤和水体中,对环境造成极大的损害,对民众的健康构成了很大的威胁,所以检测此类化合物对环境和人体健康都具有十分重要的意义。其中,硝基爆炸物是人类在军事行动和犯罪行为使用最广泛的,作为普通工业炸药,常见的有2,4,6-三硝基甲苯,2,4,6-三硝基苯酚、2,4-二硝基甲苯和三硝基苯甲硝胺。现在硝基苯的检测方法主要有气相色谱法、气质谱联用技术、电化学法,液相色谱法、表面等离子共振光谱法等。然而这些方法都存在着一定的局限性,如仪器复杂难以操作和设备昂贵导致不能广泛应用,爆炸物检测限低、灵敏度低、不能做到选择性检测、检测方法不稳定性等问题。
随着纳米科学的不断进步,纳米材料借助其独特优异的光学、电学性能成为近些年的研究热点。半导体量子点具有宽激发,强量子效率,较大的半径位移和狭窄对称的荧光谱峰,背景干扰小,荧光稳定,发光强等特点,使其在检测、细胞成像和癌症追踪的等生物学领域具有潜在的应用价值。为了实现硝基芳香族爆炸品的分析检测,设计一种简单的基于量子点发光材料的2,4,6-三硝基甲苯传感器,达到水溶性好、高灵敏度、快速且低成本的检测目的,是本发明的意义和重点所在。
发明内容
本发明的目的是提供一种光聚合法制备亲水性荧光纳米球及其在2,4,6-三硝基甲苯爆炸物痕量检测中的应用。
本发明以烯丙基硫醇修饰的硫化锌掺锰量子点为功能单体,通过紫外光辐射使其聚合得到亲水性荧光纳米球,并将其应用于2,4,6-三硝基甲苯硝基爆炸物的检测。
本发明所述的亲水性荧光纳米球的制备方法,其具体步骤如下:
a.将0.3-1.0mmol可溶解于氯仿中的硫化锌掺锰量子点、0.01-1.0mmol的烯丙基硫醇注射入4-10mL氯仿中,均匀搅拌10-30min,产物用10-30mL乙醇沉淀,离心得到白色沉淀,然后超声分散到2-6mL氯仿中,得到烯丙基硫醇修饰的硫化锌掺锰量子点分散液;
b.将5-50mg十二烷基磺酸钠加入5-15mL去离子水中完全溶解;
c.将0.1-0.8mL步骤a得到的分散液、5-50μg偶氮二异丁腈、0.2-0.9mL氯仿混合均匀后,倒入步骤b配制的十二烷基磺酸钠水溶液中,于超声波细胞破碎机中超声3-5min,得到白色微乳液;
d.将步骤c得到的白色微乳液置于紫外激光器下照射5-30min,期间在搅拌条件下滴加0.5-5.0mg的巯基乙胺;
e.最后在室温下搅拌,待氯仿完全挥发后,8000-12000r/min离心10-25min得到白色沉淀,再用去离子水离心清洗掉表面残留的十二烷基磺酸钠,最终将沉淀分散到3-5mL去离子水中,即得到亲水性荧光纳米球。所述的紫外激光器照射波长为365nm。
调控步骤a中的烯丙基硫醇的浓度在3.75-9.9mM范围内,最终得到的亲水性荧光纳米球粒径范围在50-100nm间可控调变。
将上述制备的亲水性荧光纳米球应用于2,4,6-三硝基甲苯爆炸物的痕量检测中。
本发明的有益效果:本发明采用光激发原位聚合法,将油相量子点聚合为亲水性荧光纳米球,调控烯丙基硫醇单体的变化量在3.75-9.9mM×1.0mL氯仿之间,可以得到在50-100nm间尺寸可调变的纳米球。通过该方法得到的纳米球,可以在水相中稳定分散并且尺寸均一。在2,4,6-三硝基甲苯爆炸物存在的条件下,修饰在纳米球表面的氨基与2,4,6-三硝基甲苯在强碱性条件下特异性结合,会发生电子转移,使其在350-600nm间有一宽吸收峰,在342nm近红外光的激发下,与硫化锌掺锰纳米颗粒的591nm处的发射峰发生重叠,产生有效的荧光淬灭,可以通过检测荧光强度,达到定性定量检测2,4,6-三硝基甲苯的目的。与传统的检测方法比较,该方法操作简单,背景干扰小,信号强,成本低,且具有检测限低,快速准确,灵敏度高的特点。这在功能纳米材料合成技术和硝基爆炸物检测技术方面都具有重要的意义。
附图说明
图1:实施例1制得的亲水性荧光纳米球的透射照片。
图2:实施例1制得的亲水性荧光纳米球的粒径分布图。
图3:实施例2制得的亲水性荧光纳米球的透射照片。
图4:实施例2制得的亲水性荧光纳米球的粒径分布图。
图5:实施例3制得的亲水性荧光纳米球的透射照片。
图6:实施例3制得的亲水性荧光纳米球的粒径分布图。
图7:2,4,6-三硝基甲苯硝基爆炸物在强碱条件下的紫外吸收峰。
图8:实施例3制得的亲水性荧光纳米球检测2,4,6-三硝基甲苯的荧光光谱图。
具体实施方式
实施例1
1.将0.8mmol的可溶解于氯仿中的硫化锌掺锰量子点(锰的摩尔掺杂量为5%)、0.06mmol的烯丙基硫醇注射入6mL氯仿中,均匀搅拌20min,产物用20mL乙醇沉淀,离心得到白色沉淀,然后超声分散到4mL氯仿中,得到烯丙基硫醇修饰的硫化锌掺锰量子点分散液;
2.将18mg十二烷基磺酸钠加入10mL去离子水中完全溶解;
3.将0.25mL步骤1得到的分散液、6.25μg偶氮二异丁腈、0.75mL氯仿混合均匀后,倒入步骤2配制的十二烷基磺酸钠水溶液中,于超声波细胞破碎机中超声3min,得到白色微乳液;
4.将步骤3得到的白色微乳液置于365nm紫外激光器下照射10min,期间在搅拌条件下滴加1mg巯基乙胺;
5.最后在室温下搅拌,待氯仿完全挥发后,12000r/min离心20min得到白色沉淀,再用去离子水离心清洗掉表面残留的十二烷基磺酸钠,最终将沉淀分散到3mL去离子水中,即得到亲水性荧光纳米球。
实施例2
1.将0.5mmol的可溶解于氯仿中的硫化锌掺锰量子点(锰的摩尔掺杂量为5%)、0.06mmol的烯丙基硫醇注射入6mL氯仿中,均匀搅拌20min,产物用20mL乙醇沉淀,离心得到白色沉淀,然后超声分散到4mL氯仿中,得到烯丙基硫醇修饰的硫化锌掺锰量子点分散液;
2.将18mg十二烷基磺酸钠加入10mL去离子水中完全溶解;
3.将0.40mL步骤1得到的分散液、10.0μg偶氮二异丁腈、0.60mL氯仿混合均匀后,倒入步骤2配制的十二烷基磺酸钠水溶液中,于超声波细胞破碎机中超声3min,得到白色微乳液;
4.将步骤3得到的白色微乳液置于365nm紫外激光器下照射10min,期间在搅拌条件下滴加1mg巯基乙胺;
5.最后在室温下搅拌,待氯仿完全挥发后,12000r/min离心20min得到白色沉淀,再用去离子水离心清洗掉表面残留的十二烷基磺酸钠,最终将沉淀分散到3mL去离子水中,即得到亲水性荧光纳米球。
实施例3
1.将0.3mmol油相的硫化锌掺锰量子点(锰的摩尔掺杂量为5%)、0.06mmol的烯丙基硫醇注射入6mL氯仿中,均匀搅拌20min,产物用20mL乙醇沉淀,离心得到白色沉淀,然后超声分散到4mL氯仿中,得到烯丙基硫醇修饰的硫化锌掺锰量子点分散液;
2.将18mg十二烷基磺酸钠加入10mL去离子水中完全溶解;
3.将0.66mL步骤1得到的分散液、16.5μg偶氮二异丁腈、0.34mL氯仿混合均匀后,倒入步骤2配制的十二烷基磺酸钠水溶液中,于超声波细胞破碎机中超声3min,得到白色微乳液;
4.将步骤3得到的白色微乳液置于365nm紫外激光器下照射10min,期间在搅拌条件下滴加1mg巯基乙胺;
5.最后在室温下搅拌,待氯仿完全挥发后,12000r/min离心20min得到白色沉淀,再用去离子水离心清洗掉表面残留的十二烷基磺酸钠,最终将沉淀分散到3mL去离子水中,即得到亲水性荧光纳米球。
将上述制备的亲水性荧光纳米球应用于2,4,6-三硝基甲苯爆炸物的检测:
a.配制浓度为0,0.01,0.02,0.03,0.04,0.05,0.1,0.2,0.3,0.4,0.5μg/mL 2,4,6-三硝基甲苯爆炸物溶液;
b.将步骤a配制的2,4,6-三硝基甲苯爆炸物溶液分别加入上述光聚合法制备的亲水性荧光纳米球分散液中,再加入pH=12的缓冲溶液,常温下混合均匀后进行光谱测试;
c.固定激发光波长为342nm,收集530-630nm波长范围内的光谱图。
Claims (4)
1.一种亲水性荧光纳米球的制备方法,其特征在于,其具体步骤如下:
a.将0.3-1.0mmol可溶解于氯仿中的硫化锌掺锰量子点、0.01-1.0mmol的烯丙基硫醇注射入4-10mL氯仿中,均匀搅拌10-30min,产物用10-30mL乙醇沉淀,离心得到白色沉淀,然后超声分散到2-6mL氯仿中,得到烯丙基硫醇修饰的硫化锌掺锰量子点分散液;
b.将5-50mg十二烷基磺酸钠加入5-15mL去离子水中完全溶解;
c.将0.1-0.8mL步骤a得到的分散液、5-50μg偶氮二异丁腈、0.2-0.9mL氯仿混合均匀后,倒入步骤b配制的十二烷基磺酸钠水溶液中,于超声波细胞破碎机中超声3-5min,得到白色微乳液;
d.将步骤c得到的白色微乳液置于紫外激光器下照射5-30min,期间在搅拌条件下滴加0.5-5.0mg的巯基乙胺;
e.最后在室温下搅拌,待氯仿完全挥发后,8000-12000r/min离心10-25min得到白色沉淀,再用去离子水离心清洗掉表面残留的十二烷基磺酸钠,最终将沉淀分散到3-5mL去离子水中,即得到亲水性荧光纳米球。
2.根据权利要求1所述的制备方法,其特征在于,所述的紫外激光器照射波长为365nm。
3.根据权利要求1所述的制备方法,其特征在于,调控步骤a中的烯丙基硫醇的浓度在3.75-9.9mM范围内,最终得到的亲水性荧光纳米球粒径范围在50-100nm间可控调变。
4.根据权利要求1-3任一所述的方法制备得到的亲水性荧光纳米球在检测2,4,6-三硝基甲苯爆炸物中的应用。
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