CN103592271B - 一种利用荧光纳米CdSe量子点探针检测氟氰戊菊酯农药的方法 - Google Patents
一种利用荧光纳米CdSe量子点探针检测氟氰戊菊酯农药的方法 Download PDFInfo
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Abstract
本发明公开了一种利用荧光纳米CdSe量子点探针检测氟氰戊菊酯农药的方法，基于荧光纳米CdSe量子点与氟氰戊菊酯之间的相互作用，导致荧光纳米CdSe量子点的荧光强度发生变化，可以快速检测溶液中的氟氰戊菊酯农药，对氟氰戊菊酯农药的检测限可达到5.1×10–8mol/L。本发明方法操作简单方便、检测快速且选择性好，在混合样品中进行氟氰戊菊酯检测时具有高灵敏和高选择性的特点。
Description
技术领域
本发明属于氟氰戊菊酯农药检测技术领域，具体涉及一种利用荧光纳米CdSe量子点探针检测氟氰戊菊酯农药的方法。
背景技术
氟氰戊菊酯属于菊酯类农药，是一种中等毒性杀虫剂。氟氰戊菊酯以触杀和胃毒为主，没有熏蒸和内吸作用，是一种杀虫谱广、药效迅速的广谱杀虫剂。可有效用于棉花、蔬菜、果树等作物上防治鳞翅目，同翅目、双翅目、鞘翅目等多种害虫，对叶螨也有一定抑制作用。氟氰戊菊酯可与一般杀虫剂、杀菌剂混用，对鱼类、蜜蜂有剧毒。截至目前，氟氰戊菊酯农药的检测方法主要有色谱法和免疫法这两大类，但这两类方法往往具有操作繁琐、成本高等不足。因此，建立简便且灵敏度高的氟氰戊菊酯农药检测方法逐渐成为研究热点。
近些年，荧光纳米CdSe量子点作为一种荧光探针，逐渐引起人们的关注。与传统的有机荧光染料和荧光蛋白相比，量子点具有发射光谱窄而对称、荧光量子产率高、抗光漂白性能强等优越的光谱性质，并被广泛应用于生化分析检测。但是，利用量子点CdSe荧光探针检测氟氰戊菊酯农药的报道几乎未见。
针对以上问题，我们研究了一种利用荧光纳米CdSe量子点探针检测氟氰戊菊酯农药的新方法，该方法操作简单快速、检测灵敏度高。
发明内容
本发明的目的在于提供一种利用荧光纳米CdSe量子点探针检测氟氰戊菊酯农药的方法。
本发明解决上述技术问题的技术方案如下：
1.荧光纳米CdSe量子点探针的制备方法如下：
称取0.03g硒粉加入到装有0.22g三正丁基膦和1.2g二辛基胺的烧瓶中，静置12h，制备硒储备液；取0.012g氧化镉和0.12g硬脂酸于三口烧瓶中，氩气保护下加热至162℃使氧化镉充分溶解，制备镉储备液；在制好的镉储备液中加入1.2g三正辛基氧膦和1.2g十六胺，氩气保护下搅拌并加热至302℃，取出的硒储备液注入到反应容器中，继续在282℃反应70秒，使产物冷却至室温后，即制得荧光纳米CdSe量子点探针。
2.利用步骤1制备的荧光纳米CdSe量子点探针检测氟氰戊菊酯农药的方法：
应用荧光纳米CdSe量子点探针检测氟氰戊菊酯农药时，将稀释15倍后的荧光纳米CdSe量子点探针溶液与氟氰戊菊酯农药溶液混合，并使荧光纳米CdSe量子点探针溶液与氟氰戊菊酯农药溶液的摩尔比为1∶0.66～16，从荧光光谱图可得知荧光纳米CdSe量子点探针的荧光强度随氟氰戊菊酯农药的浓度的增加而减弱，且荧光强度与氟氰戊菊酯农药浓度之间呈良好的线性关系，相关系数为0.9999，因此，荧光纳米CdSe量子点探针可以作为检测氟氰戊菊酯农药的探针快速并定量检测正己烷溶液中氟氰戊菊酯农药的含量，对氟氰戊菊酯农药的检测限可达到5.1×10–8mol/L。
本发明的优点：
1.本发明提供的荧光纳米CdSe量子点探针荧光性能好、荧光强度高。
2.采用本发明所制备的荧光纳米CdSe量子点探针对氟氰戊菊酯农药进行检测，具有简单方便、灵敏度高、检测限低的特点。
附图说明
图1是本发明的荧光纳米CdSe量子点探针在氟氰戊菊酯农药检测过程中，不同氟氰戊菊酯农药浓度与荧光纳米CdSe量子点探针反应后，激发波长为380nm时所得到的荧光光谱图；
图中，a～e为实施例中加入的不同氟氰戊菊酯农药浓度，使探针与氟氰戊菊酯农药的摩尔比为1∶0.66～16的荧光光谱图。
具体实施方式
为了更好的理解本发明，下面结合具体的实施例对本发明做进一步的详细阐述。应理解，以下实施例只是本发明的一些优选实施方式，目的在于更好地阐述本发明的内容，而不是对本发明的保护范围产生任何限制。
实施例1
荧光纳米CdSe量子点探针的制备：
称取0.03g硒粉加入到装有0.22g三正丁基膦和1.2g二辛基胺的烧瓶中，静置12h，制备硒储备液；取0.012g氧化镉和0.12g硬脂酸于三口烧瓶中，氩气保护下加热至162℃使氧化镉充分溶解，制备镉储备液；在制好的镉储备液中加入1.2g三正辛基氧膦和1.2g十六胺，氩气保护下搅拌并加热至302℃，取出的硒储备液注入到反应容器中，继续在282℃反应70秒，使产物冷却至室温后，即制得荧光纳米CdSe量子点探针。
实施例2
一种利用荧光纳米CdSe量子点探针检测氟氰戊菊酯农药的方法：
应用荧光纳米CdSe量子点检测氟氰戊菊酯农药标准品中氟氰戊菊酯农药的过程中，将稀释15倍后的荧光纳米CdSe量子点探针溶液与氟氰戊菊酯农药溶液混合，其中，荧光纳米CdSe量子点探针溶液与氟氰戊菊酯农药溶液的摩尔比为1∶0.66，即得到图1中荧光光谱a。
实施例3
一种利用荧光纳米CdSe量子点探针检测氟氰戊菊酯农药的方法：
其余条件均与步骤1相同，仅荧光纳米CdSe量子点探针溶液与氟氰戊菊酯农药溶液的摩尔比改为1∶3.3，则得到图1中荧光光谱b。
实施例4
一种利用荧光纳米CdSe量子点探针检测氟氰戊菊酯农药的方法：
其余条件均与步骤1相同，仅荧光纳米CdSe量子点探针溶液与氟氰戊菊酯农药溶液的摩尔比改为1∶5.9，则得到图1中荧光光谱c。
实施例5
一种利用荧光纳米CdSe量子点探针检测氟氰戊菊酯农药的方法：
其余条件均与步骤1相同，仅荧光纳米CdSe量子点探针溶液与氟氰戊菊酯农药溶液的摩尔比改为1∶9.5，则得到图1中荧光光谱d。
实施例6
一种利用荧光纳米CdSe量子点探针检测氟氰戊菊酯农药的方法：
其余条件均与步骤1相同，仅荧光纳米CdSe量子点探针溶液与氟氰戊菊酯农药溶液的摩尔比改为1∶16，则得到图1中荧光光谱e。
从以上实施例荧光光谱图1可得知荧光纳米CdSe量子点探针的荧光强度随氟氰戊菊酯农药的浓度的增加而减弱，且荧光强度的降低值与氟氰戊菊酯农药浓度有良好的线性关系，R2=0.9999。
Claims (1)
1.一种利用荧光纳米CdSe量子点探针检测氟氰戊菊酯农药的方法，其特征在于，
1)荧光纳米CdSe量子点探针的制备：
称取0.03g硒粉加入到装有0.22g三正丁基膦和1.2g二辛基胺的烧瓶中，静置12h，制备硒储备液；取0.012g氧化镉和0.12g硬脂酸于三口烧瓶中，氩气保护下加热至162℃使氧化镉充分溶解，制备镉储备液；在制好的镉储备液中加入1.2g三正辛基氧膦和1.2g十六胺，氩气保护下搅拌并加热至302℃，取出的硒储备液注入到反应容器中，继续在282℃反应70秒，使产物冷却至室温后，即制得荧光纳米CdSe量子点探针；
2)利用步骤1)制备的荧光纳米CdSe量子点探针检测氟氰戊菊酯农药的方法：
将稀释15倍后的荧光纳米CdSe量子点探针溶液与氟氰戊菊酯农药溶液混合，并使荧光纳米CdSe量子点探针溶液与氟氰戊菊酯农药溶液的摩尔比为1∶0.66～16，从荧光光谱图可得知荧光纳米CdSe量子点探针的荧光强度随氟氰戊菊酯农药的浓度的增加而减弱，且荧光强度与氟氰戊菊酯农药浓度之间呈良好的线性关系，相关系数为0.9999，因此，荧光纳米CdSe量子点探针可以作为检测氟氰戊菊酯农药的探针快速并定量检测正己烷溶液中氟氰戊菊酯农药的含量，对氟氰戊菊酯农药的检测限可达到5.1×10–8mol/L。
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