CN103592274B - 一种利用荧光纳米CdSe量子点探针检测联苯菊酯农药的方法 - Google Patents
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Abstract
本发明公开了一种利用荧光纳米CdSe量子点探针检测联苯菊酯农药的方法，基于联苯菊酯能有效猝灭荧光纳米CdSe量子点探针的荧光，因此可以利用荧光猝灭现象快速灵敏检测溶液中的联苯菊酯农药，对联苯菊酯农药的检测限可达到5.1×10–8mol/L，相关系数为0.9999。本发明方法不仅操作简单方便，而且灵敏度高、选择性好，可实现混合样品中联苯菊酯的高灵敏和高选择性的检测。
Description
技术领域
本发明属于联苯菊酯农药检测技术领域，具体涉及一种利用荧光纳米CdSe量子点探针检测联苯菊酯农药的方法。
背景技术
联苯菊酯属于一种拟除虫菊酯类杀虫杀螨剂，杀虫活性很高，主要为触杀和胃毒作用，不存在熏蒸和内吸作用。联苯菊酯是一种广谱杀虫剂，对蜜蜂毒性中等，对家蚕毒性较高。联苯菊酯作用于昆虫时具有作用迅速、持效期长的特点，对许多害虫和多种叶螨同时具有良好的防治效果，但对鱼毒性很高。截至目前为止，主要采用色谱法和免疫法进行联苯菊酯农药的检测，但这两类方法存在操作繁琐、成本高的缺点。因此，建立操作简便、简单易行的联苯菊酯农药检测方法已成为当今发展趋势。
近年来，荧光纳米CdSe量子点探针逐渐引起了科研工作者们的广泛关注。相比传统的有机荧光染料和荧光蛋白，量子点具有许多优越的光谱性质，如激发光谱宽、发射光谱窄而对称、荧光量子产率高、荧光稳定性强、抗光漂白性能强等，这些优越的光谱性质使荧光纳米CdSe量子点探针被广泛应用于生化分析领域。然而，迄今为止，采用荧光纳米CdSe量子点探针检测联苯菊酯农药的报道尚未见。
针对以上问题，我们研究了一种利用荧光纳米CdSe量子点探针检测联苯菊酯农药的新方法，该方法操作简单、灵敏度高、选择性好，能用于混合溶液中联苯菊酯的高灵敏检测。
发明内容
本发明的目的在于提供一种利用荧光纳米CdSe量子点探针检测联苯菊酯农药的方法。
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0.05g硒粉加入到装有0.28g三正丁基膦和1.4g二辛基胺的烧瓶中，静置14h，制备硒储备液；取0.018g氧化镉和0.15g硬脂酸于三口烧瓶中，氩气保护下加热至168℃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1.34g三正辛基氧膦和1.4g十六胺，氩气保护下搅拌并加热至308℃，取出的硒储备液注入到反应容器中，继续在288℃反应90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量子点探针检测联苯菊酯农药的方法：
应用荧光纳米CdSe量子点探针检测联苯菊酯农药时，将稀释25倍后的荧光纳米CdSe量子点探针溶液与联苯菊酯农药溶液混合，并将荧光纳米CdSe量子点探针溶液与联苯菊酯农药溶液的摩尔比控制在1∶0.71～18的范围内，此时联苯菊酯能有效猝灭荧光纳米CdSe量子点探针的荧光，且荧光纳米CdSe量子点探针的荧光强度与联苯菊酯农药浓度之间呈良好的线性关系，因此，荧光纳米CdSe量子点探针可以作为检测联苯菊酯农药的探针，并能快速灵敏检测正己烷溶液中联苯菊酯农药的含量，对联苯菊酯农药的检测限为5.1×10–8mol/L。
本发明的优点：
1.本发明提供的荧光纳米CdSe量子点探针荧光强度高、荧光稳定性高、抗光漂白性能强。
2.采用本发明所制备的荧光纳米CdSe量子点探针对联苯菊酯农药进行检测，具有操作简便、灵敏度高、选择性好的优点。
附图说明
图1是本发明的荧光纳米CdSe量子点探针在联苯菊酯农药检测过程中，不同联苯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388nm时所得到的荧光光谱图；
图中，a～e为实施例中加入的不同联苯菊酯农药浓度，使探针与联苯菊酯农药的摩尔比为1∶0.71～18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0.05g硒粉加入到装有0.28g三正丁基膦和1.4g二辛基胺的烧瓶中，静置14h，制备硒储备液；取0.018g氧化镉和0.15g硬脂酸于三口烧瓶中，氩气保护下加热至168℃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1.34g三正辛基氧膦和1.4g十六胺，氩气保护下搅拌并加热至308℃，取出的硒储备液注入到反应容器中，继续在288℃反应90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量子点探针检测联苯菊酯农药的方法：
应用荧光纳米CdSe量子点检测联苯菊酯农药标准品中联苯菊酯农药的过程中，将稀释25倍后的荧光纳米CdSe量子点探针溶液与联苯菊酯农药溶液混合，使荧光纳米CdSe量子点探针溶液与联苯菊酯农药溶液的摩尔比为1∶0.71，即得到图1中荧光光谱a。
实施例3
一种利用荧光纳米CdSe量子点探针检测联苯菊酯农药的方法：
其余条件均与步骤1相同，仅荧光纳米CdSe量子点探针溶液与联苯菊酯农药溶液的摩尔比改为1∶2.8，则得到图1中荧光光谱b。
实施例4
一种利用荧光纳米CdSe量子点探针检测联苯菊酯农药的方法：
其余条件均与步骤1相同，仅荧光纳米CdSe量子点探针溶液与联苯菊酯农药溶液的摩尔比改为1∶5.6，则得到图1中荧光光谱c。
实施例5
一种利用荧光纳米CdSe量子点探针检测联苯菊酯农药的方法：
其余条件均与步骤1相同，仅荧光纳米CdSe量子点探针溶液与联苯菊酯农药溶液的摩尔比改为1∶10，则得到图1中荧光光谱d。
实施例6
一种利用荧光纳米CdSe量子点探针检测联苯菊酯农药的方法：
其余条件均与步骤1相同，仅荧光纳米CdSe量子点探针溶液与联苯菊酯农药溶液的摩尔比改为1∶18，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联苯菊酯农药的浓度的增加而减弱，且荧光强度的降低值与联苯菊酯农药浓度之间有良好的线性关系，R2=0.9999。
Claims (1)
1.一种利用荧光纳米CdSe量子点探针检测联苯菊酯农药的方法，其特征在于，
1)荧光纳米CdSe量子点探针的制备：
称取0.05g硒粉加入到装有0.28g三正丁基膦和1.4g二辛基胺的烧瓶中，静置14h，制备硒储备液；取0.018g氧化镉和0.15g硬脂酸于三口烧瓶中，氩气保护下加热至168℃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1.34g三正辛基氧膦和1.4g十六胺，氩气保护下搅拌并加热至308℃，取出的硒储备液注入到反应容器中，继续在288℃反应90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量子点探针检测联苯菊酯农药的方法：
将稀释25倍后的荧光纳米CdSe量子点探针溶液与联苯菊酯农药溶液混合，并将荧光纳米CdSe量子点探针溶液与联苯菊酯农药溶液的摩尔比控制在1∶0.71～18的范围内，此时联苯菊酯能有效猝灭荧光纳米CdSe量子点探针的荧光，且荧光纳米CdSe量子点探针的荧光强度与联苯菊酯农药浓度之间呈良好的线性关系，因此，荧光纳米CdSe量子点探针可以作为检测联苯菊酯农药的探针，并能快速灵敏检测正己烷溶液中联苯菊酯农药的含量，对联苯菊酯农药的检测限为5.1×10–8mol/L。
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