背景:目前已经对金属离子化磷酸锆的制备及抗菌活性进行了系统研究,但易变色或抗菌活性不足的缺点限制了它们的广泛应用。课题组拟将高效、广谱、低毒季铵盐杀菌剂通过离子交换法负载在磷酸锆钠上希望能够制备出颜色稳定、抗菌活性高的新型季铵化磷酸锆抗菌剂。目的:分析季铵化磷酸锆的组成结构和抗菌活性。设计、时间及地点:体外观察实验,于2009-06/08在暨南大学化学系科研实验室完成。材料:采用离子交换法将十二烷基二甲基苄基氯化铵引入磷酸锆钠中制备季铵化磷酸锆。方法:反应体系中按季铵阳离子与磷酸锆钠的阳离子交换容量的摩尔比分别为0.25︰1,0.5︰1,1.0︰1和1.5︰1加料,采用离子交换法制备了4种不同季铵阳离子含量的季铵化磷酸锆(QZrP-1,QZrP-2,QZrP-3,QZrP-4)。主要观察指标:分别通过红外光谱仪,元素分析仪,热分析仪分析样品的组成结构和热稳定性。采用试管稀释法测定样品对大肠杆菌和金黄色葡萄球菌的最低抑菌浓度和最低杀菌浓度。结果:季铵化磷酸锆中结合了季铵阳离子,其含量随着反应液中季铵盐添加量的增加而增加。季铵化磷酸锆QZrP-1、QZrP-2、QZrP-3、QZrP-4中季铵阳离子的质量分数分别为3.70%、5.00%、6.96%和10.01%。季铵化磷酸锆中季铵阳离子的热分解起始温度都大于345 ℃,具有良好的热稳定性。随着季铵阳离子含量的增加,季铵化磷酸锆的抗菌活性增强。所制备的季铵阳离子质量分数为6.96%的QZrP-3样品,其对E. coli、S. aureus都显示出良好的抗菌活性。结论:季铵阳离子质量分数为6.96%的季铵化磷酸锆(QZrP-3)热稳定性好、抗菌活性高。
BACKGROUND: The preparation and antibacterial activity of metal ionic zirconium phosphates has been systemically investigated now, but the applications are limited owing to the discoloration or the low antibacterial activity. Here we prepared new antibacterial agents of quaternized zirconium phosphates by introducing quaternary ammonium salt bactericidal agent with high-effective, broad-spectrum and low-toxic into sodium zirconium phosphate through an ion-exchange method. OBJECTIVE: To explore the component structure and antibacterial activity of quaternized zirconium phosphates. DESIGN, TIME AND SETTING: An in vitro observational experiment was performed at Research Laboratory of Department of Chemistry, Jinan University from June to August 2009. MATERIALS: Quaternized zirconium phosphates were prepared by introducing dodecyl dimethyl benzyl ammonium chloride into sodium zirconium phosphate through an ion-exchange method. METHODS: The mol ratios of quaternary ammonium cations to cation exchange capacity of sodium zirconium phosphate in reaction solutions were 0.25︰1, 0.5︰1,1.0︰1, and 1.5︰1, respectively, and four kinds of quaternized zirconium phosphates containing different contents of quaternary ammonium cations (QZrP-1, QZrP-2, QZrP-3, QZrP-4) were prepared through an ion-exchange method. MAIN OUTCOME MEASURES: The component structure and heat resistance of samples were measured by using an IR spectrometer, an elemental analyzer and a thermal analyzer, respectively. The minimum inhibitory concentrations (MICs) and minimal bactericidal concentrations (MICs) of the samples against Escherichia coli (E. coli) and Staphylococci aureus (S. aureus) were estimated by a tube broth method. RESULTS: Quaternized zirconium phosphates were prepared, and the quaternary ammonium cation content increased with increasing the concentration of quaternary ammonium cations in reaction solution. The mass fraction of quaternary ammonium cations of QZrP-1, QZrP-2, QZrP-3, and QZrP-4 was 3.70%