CN107141310A - 一种新型抗菌锌配合物的制备方法及其应用 - Google Patents
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Abstract
本发明公开了一种新型抗菌锌配合物,属于抗菌配合物制备方法及其应用技术领域。制备方法为:利用溶剂挥发法,在95%乙醇中,1,1'‑(吡啶‑2,5‑二基)双苯并咪唑与七水合硫酸锌作用,得到具有抗菌活性的新型含金属锌的配合物,该属于三斜晶系,空间群为Pī,晶胞参数为:a=15.706(6)Å,b=16.114(6)Å,c=17.160(7)Å,a=91.418(7)°,β=115.716(7)°,γ=103.594(7)°,V=3763(2)Å3。不对称单元中包含两个Zn(II)离子、四个PBBI(1,1'‑(吡啶‑2,5‑二基)双苯并咪唑)、两个硫酸根、四个配位水分子和5个未配位水分子,Zn1和Zn2分别与来自两个PBBI配体中的氮原子、两个硫酸根中的氧原子和两个水分子中的氧原子配位,形成扭曲的八面体。本发明提出的一种新型抗菌锌配合物,合成方法简单、操作简便、稳定性强,能够有效抑制革兰阴性菌大肠杆菌(ATCC25922)、铜绿假单胞菌和革兰阳性菌金黄色葡萄球菌(ATCC25923),具有可进一步开发应用前景。
Description
技术领域
本发明涉及配合物制备方法及其应用技术领域,尤其是涉及一种抗菌配合物的制备方法及其应用。
背景技术
长期以来,由于滥用抗生素导致细菌耐药,产生所谓的“超级细菌”,已成为一个全球医疗卫生难题,使得临床抗菌药物受到了极大的挑战,合成新型抗菌药是解决当前细菌多药耐药性的关键。配合物能够有效催化细菌细胞膜发生过氧化作用,破坏细菌细胞膜,从而导致细菌死亡而达到抗菌作用。因此,构筑新型配合物作为抗菌药物是解决细菌耐药性问题的重要途径之一,配合物作为抗菌药具有显著的优势。
基于上述原因,本发明人制备了一种新型抗菌锌配合物,具有良好的体外抗菌活性,能够有效抑制革兰阴性菌大肠杆菌(ATCC25922)、铜绿假单胞菌和革兰阳性菌金黄色葡萄球菌(ATCC25923)。
发明内容
本发明的目的在于提供一种新型抗菌锌配合物的制备方法,其合成方法简单、操作简便、稳定性强以及抗菌活性较强。
本发明的目的是通过如下技术方案实现的:一种新型抗菌锌配合物,分子式为Zn2(PBBI)4(SO4)2(H2O)2·5H2O,其中,PBBI为1,1'-(吡啶-2,5-二基)双苯并咪唑,其结构式为:。
所述一种新型抗菌锌配合物属于三斜晶系,空间群为Pī,晶胞参数为:a = 15.706(6)Å, b = 16.114(6)Å,c = 17.160(7)Å,a = 91.418(7)°,β = 115.716(7)°,γ =103.594(7)°,V = 3763(2)Å3。
所述一种新型抗菌锌配合物的基本结构单元中包含两个Zn(II)离子、四个PBBI(1,1'-(吡啶-2,5-二基)双苯并咪唑)、两个硫酸根、四个配位水分子和5个未配位水分子。Zn1和Zn2分别与来自两个PBBI配体中的氮原子、两个硫酸根中的氧原子和两个水分子中的氧原子配位,形成扭曲的八面体,该配合物中其中一个硫酸根存在无序情况。
所述一种新型抗菌锌配合物的制备方法:称取0.0125 mmol配体1,1'-(吡啶-2,5-二基)双苯并咪唑超声溶解于95%乙醇中,再称取0.0125mmol七水合硫酸锌超声溶解于95%乙醇中,将两种溶液充分混合,再超声10-20min,过滤,滤液于室温下缓慢挥发溶剂,一周后得到无色块状晶体,收集晶体,依次经过95%乙醇洗涤、干燥处理,得到目标物。
所述一种新型抗菌锌配合物具有良好的抗菌效果,对革兰阴性菌大肠杆菌(ATCC25922)、铜绿假单胞菌和革兰阳性菌金黄色葡萄球菌(ATCC25923)表现出较强的抑制作用。
本发明的有益效果是:本发明提出的一种新型抗菌锌配合物,合成方法简单、操作简便、稳定性强,能够有效抑制革兰阴性菌大肠杆菌(ATCC25922)、铜绿假单胞菌和革兰阳性菌金黄色葡萄球菌(ATCC25923)。本发明提出的一种新型抗菌锌配合物作为抗菌剂具有可进一步开发应用前景。
附图说明
图1为本发明所提出的一种新型抗菌锌配合物的结构图,为了清晰起见,省略了氢原子和未配位溶剂分子。
图2为本发明所提出的一种新型抗菌锌配合物的X-粉末衍射图谱。
图3为本发明所提出的一种新型抗菌锌配合物的热重曲线图。
具体实施方式
下面结合具体实施方式对本发明作进一步说明,需说明的是,本发明要求保护的范围并不局限于实施例表述的范围。
所述一种新型抗菌锌配合物的制备方法:称取1,1'-(吡啶-2,5-二基)双苯并咪唑(0.0125 mmol,3.89mg)超声溶解于5 mL 95%乙醇中,再称取七水合硫酸锌(0.0125 mmol,3.59mg)超声溶解于5 mL 95%乙醇中,然后将两种溶液充分混合,再超声振荡10-20min,过滤,滤液置于小试管中,用保鲜膜封住试管口,在保鲜膜上用针扎几个小孔,于室温下缓慢挥发溶剂,一周后得到无色块状晶体,收集晶体,晶体用95%乙醇洗涤,干燥,得到目标物,产率约56%。
所述配合物的晶体结构表征为:选取大小合适的单晶在室温下进行X-射线衍射实验。单晶X-射线数据是由石墨单色器Mo Kα(λ = 0.71073 Å)作为放射源,在Bruker APEX-II CCD单晶衍射仪上采集的,所得到的数据都应用了经验吸收校正。晶体结构采用SHELXTL-97 程序通过直接法解出,运用F 2全矩阵最小二乘方法进行了精修。所有的非氢原子的各向异性都进行了精修,所有氢原子的位置都是通过计算得到的。配合物的晶体学数据和结构精修结果列于表1中,部分键长和键角列于表2中,配合物的结构见图1。
表1 配合物的主要晶体学数据和结构精修结果
R 1 =ΣllF0l-lFcll/ΣlF0l; wR 2 =Σ[w(F0 2–FC 2)2]/ Σ[w(F0 2)2]1/2
表2配合物的部分键长(Å)和键角(º)
Zn(1)-O(6) 2.095(6) | Zn(1)-O(3) 2.096(5) |
Zn(1)-N(6) 2.111(6) | Zn(1)-O(2W) 2.119(5) |
Zn(1)-O(1W) 2.127(6) | Zn(1)-N(1) 2.134(7) |
Zn(2)-O(4W) 2.085(6) | Zn(2)-N(16) 2.108(6) |
Zn(2)-N(11) 2.128(6) | Zn(2)-O(2) 2.130(5) |
Zn(2)-O(7) 2.130(8) | Zn(2)-O(3W) 2.145(7) |
O(3)-Zn(1)-O(1W) 83.8(2) | O(3)-Zn(1)-N(6) 174.6(3) |
O(2)-Zn(2)-O(7) 84.6(3) | O(4W)-Zn(2)-O(3W) 175.3(2) |
所述配合物X-粉末衍射(PXRD)图谱与模拟图谱吻合较好,说明该配合物为纯相,为其作为抗菌剂的应用提供了保证,配合物的X-粉末衍射(PXRD)图谱见图2,所用仪器为TD-3500 X-粉末衍射仪。
所述配合物在100-240°发生第一次失重,失去未配位水分子,未配位水分子的失去不会导致整体结构的变化。500°以后开始骨架分解。因此在500°以内其结构稳定。(仪器型号:NETZSCH5 STA 449C)。
由上述结构表征可知,所述配合物属于三斜晶系,空间群为Pī,晶胞参数为:a =15.706(6)Å, b = 16.114(6)Å,c = 17.160(7)Å,a = 91.418(7)°,β = 115.716(7)°,γ =103.594(7)°,V = 3763(2)Å3。不对称单元中包含两个Zn(II)离子、四个PBBI(1,1'-(吡啶-2,5-二基)双苯并咪唑)、两个硫酸根、四个配位水分子和5个未配位水分子。Zn1和Zn2分别与来自两个PBBI配体中的氮原子、两个硫酸根中的氧原子和两个水分子中的氧原子配位,形成扭曲的八面体。
所述配合物的体外抗菌活性测试按照美国国家实验室标准委员会(NCCLS)推荐的标准测试方法进行,测试菌种为革兰阴性菌大肠杆菌(ATCC25922)、铜绿假单胞菌和革兰阳性菌金黄色葡萄球菌(ATCC25923)。
体外抗菌活性测试结果表明,所述配合物对大肠杆菌(ATCC25922)的MIC为32mg/mL,对铜绿假单胞菌的MIC为16mg/mL,对金黄色葡萄球菌(ATCC25923)的MIC为16mg/mL。
Claims (3)
1.一种新型抗菌锌配合物,其特征在于:分子式为Zn2(PBBI)4(SO4)2(H2O)2·5H2O,其中,PBBI为1,1'-(吡啶-2,5-二基)双苯并咪唑,配合物的结构为:
;
其中结构单元中包含两个Zn(II)离子、四个PBBI(1,1'-(吡啶-2,5-二基)双苯并咪唑)、两个硫酸根、四个配位水分子和5个未配位水分子,Zn1和Zn2分别与来自两个PBBI配体中的氮原子、两个硫酸根中的氧原子和两个水分子中的氧原子配位,形成扭曲的八面体。
2.根据权利要求1所述一种新型抗菌锌配合物的制备方法,其特征在于:称取0.0125mmol配体1,1'-(吡啶-2,5-二基)双苯并咪唑超声溶解于95%乙醇中,再称取0.0125mmol七水合硫酸锌超声溶解于95%乙醇中,将两种溶液充分混合,再超声10-20min,过滤,滤液于室温下缓慢挥发溶剂,一周后得到无色块状晶体,收集晶体,依次经过95%乙醇洗涤、干燥处理,得到目标物。
3.根据权利要求1所述一种新型抗菌锌配合物,其特征在于:具有良好的体外抗菌活性,其中对大肠杆菌(ATCC25922)的MIC为32mg/mL,对铜绿假单胞菌的MIC为16mg/mL,对金黄色葡萄球菌(ATCC25923)的MIC为16mg/mL。
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