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复方邻苯二甲醛纳米乳的研制

Studies on the Compound OPA Nanoemulsion

【作者】 韩菲

【导师】 欧阳五庆;

【作者基本信息】 西北农林科技大学 , 生理学, 2009, 硕士

【摘要】 本研究以纳米乳为载体,将邻苯二甲醛和癸甲溴铵两种消毒剂成分进行复配,旨在开发一种高效、安全、稳定的复合消毒剂,用于环境消毒。在建立分析方法、筛选处方的基础上制备出复方邻苯二甲醛纳米乳,并对其理化性质、安全性和杀菌性能进行了较为系统的研究。试验一:复方邻苯二甲醛纳米乳分析方法的建立。以邻苯二甲醛为复方邻苯二甲醛纳米乳测定的指标性成分,通过紫外分光光度法测定邻苯二甲醛的含量。建立复方邻苯二甲醛纳米乳的紫外分析方法,并对其回收率、精密度等进行研究。结果表明,以265nm作为紫外检测波长,得到的标准曲线方程为:A=0.0078C-0.0126(r=0.9998),该方程在20~100μg/mL浓度范围内,线性关系良好,平均回收率为99.16%,回收率的相对标准偏差(RSD)为0.75%、进样重复性的RSD为0.68%、日内精密度和日间精密度的RSD均小于1%。本研究建立的分析方法回收率高、精密度和重复性良好,可满足其质量控制研究。试验二:复方邻苯二甲醛纳米乳的制备。利用纳米乳的评价标准,初步筛选纳米乳处方,同时利用伪三元相图对纳米乳形成的影响因素进行考察,筛选出复方邻苯二甲醛纳米乳的最佳处方是:表面活性剂为癸甲溴铵,助表面活性剂为1,2-丙二醇,油相为IPM,表面活性剂与助表面活性剂比例(Km)为4:1,混合表面活性剂与油相比例为9:1,同时加入0.05%的离子螯合剂。本研究筛选的复方邻苯二甲醛纳米乳的制备方法简单,易于操作。试验三:复方邻苯二甲醛纳米乳的质量及稳定性评价。利用透射电镜、激光粒度分析仪对其形态和粒径进行检测;通过染色法确定纳米乳类型;通过紫外分光光度法测定邻苯二甲醛的含量;通过离心、加速试验对其稳定性进行评价。制备的复方邻苯二甲醛纳米乳为澄清透明液体,为水包油型纳米乳;在透射电镜下呈球形、粒径分布均匀,平均粒径48.2nm;邻苯二甲醛含量为:87.26mg·mL-1;离心和恒温加速试验显示其质量稳定。试验四:复方邻苯二甲醛纳米乳的杀菌性能研究。通过悬液定量杀菌试验考察不同浓度的复方邻苯二甲醛纳米乳的杀菌能力,同时考察了PH值以及有机干扰物对杀菌效能的影响。结果表明:在PH为7.2条件下含OPA 50mg/L的复方邻苯二甲醛纳米乳消毒液作用1min即可杀灭大肠杆菌和金黄色葡萄球菌(杀灭对数值>5):碱性条件有利于杀菌作用的发挥;有机干扰物对杀菌作用有一定影响。试验五:复方邻苯二甲醛纳米乳的安全性与金属腐蚀性研究。通过急性毒性、皮肤和眼部刺激试验对复方邻苯二甲醛纳米乳的安全性进行评价,同时研究该纳米乳消毒剂对金属的腐蚀性。结果表明,复方邻苯二甲醛纳米乳对小鼠的LD50>5000mg/kg.bw,属于无毒级;对家兔皮肤和眼部均无刺激,对铜和不锈钢基本无腐蚀:对碳钢和铝有轻度腐蚀。本研究制备的复方邻苯二甲醛纳米乳安全性良好,对金属腐蚀性低。试验六:复方邻苯二甲醛纳米乳的消毒模拟现场试验。结果显示:含邻苯二甲醛50mg/L的复方邻苯二甲醛纳米乳消毒剂可有效杀灭环境中99.96%的细菌。此浓度的消毒剂消毒效果良好,能满足现场消毒的需要。

【Abstract】 In this research,two disinfectant ingredients OPA and DDAB were made duplicate matches by using nanoemulsion as a new carrier.It was purposed to develop a new effective, safe and stable disinfectant for surrounding sterization.Compound OPA nanoemulsion was prepared on the base of establishment of analytical method,screening of nanoemulsion prescription and so on.Physics and chemistry nature,security and germicidal efficentcies were systemically studied.Part 1:The establishment of analytical method of compound OPA nanoemulsion.OPA was determined as content of compound OPA nanoemulsion.Establishing the Ultraviolet analytical methed of compound OPA nanoemulsion to study the recovery rate and accuracy. Results showed that OPA has the maximal absorption in 265nm.The standard curve was A=0.0078C—0.0126(r=0.9998).The good linear range was 20~100μg/mL.The average recovery rate was 99.16%.RSD of the recovery rate and repeatability were 0.75%and 0.68%. The inter-day and intra-day precision of determination of matrin is less than 1%.The analytical method in this study has high recovery,good accuracy and repeatability,which can satisfy quality control research.Part 2:The preparation of compound OPA nanoemulsion.Prescriptions of nanoemulsion were filtrated by the nanoemulsion evaluation standard.The influence factors of forming nanoemulsion were also investigated by pseudoternary phase diagrams.Results showed that the best prescriptions of the nanoemulsion were:the surfactant,cosurfactant and the oil phase were DDAB,1,2-Propylene glycol and IPM,respectively;The ratio of surfactant to cosurfactant was 4:1 and the mixed surfactant to oil was 9:1;0.05%EDTA was added.The preparation method of compound OPA nanoemulsion was simple and easy to manipulate.Part 3:The evaluation of stability and quality of compound OPA nanoemulsion.The appearance and diameter was detected by Transmission Electron Microscope(TEM) and Zetasizer Nano ZS testing.The content of OPA in nanoemulsion was tested by ultraviolet analytical methed.The stability was evaluated by centrifuging and acceleration experiments. The results showed that the compound OPA nanoemulsion was clarified and transparent liquid.Its type was O/W.Its average diameter was 48.2 nm and the content of OPA in nanoemulsion was 87.26 mg·mL-1.The quality of compound OPA nanoemulsion was stable.Part 4:Study on the germicidal efficacy of compound OPA nanoemulsion.The suspension test was conducted to learn efficacies of OPA nanoemulion in different concentration. Tests of PH and organic influential factor were also conducted.Results showed that when 50mg/L OPA in the compound OPA nanoemulsion had been for 1 minute at PH value of 7.2,The logarithm mean reduction was more the 5 against E.coli and S.aureus.The alkaline OPA nanoemulion is better for disinfection,organic substance influences its efficacy.Part 5:The safety evaluation and corrosive effect of compound OPA nanoemulsion.Safety of compound OPA nanoemulsion was evaluated by acute toxicity,skin irritation and eye irritation.It showed that the accumulation LD50 of the compound OPA nanoemulsion test on mice was more than 5000mg/kg.bw.The stimulation to the skin and eye of domestic rabbits were all nontoxic.It was not corrosive to copper and stainless steel,slight corrosive to carbon and aluminum.The compound OPA nanoemulsion is actually nontoxic and light corrosive and can be used for disinfection.Part 6:The disinfection simulated field test of compound OPA nanoemulion.Results showed that compound OPA nanoemulsion containing 50mg/L OPA can kill 99.96% bacterials in the environment.This concentration of the disinfectant had good disinfectant efficency which can satisfy our use.

【关键词】 纳米乳伪三元相图邻苯二甲醛癸甲溴铵
【Key words】 nanoemulsionpseudoternary phase diagramOPADDAB
  • 【分类号】TQ244.1
  • 【被引频次】1
  • 【下载频次】82
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