【摘要】：原位聚合法是一種制備微囊的新方法。它以芯材物質(zhì)為分散相,把可溶性預(yù)聚體與酸性催化劑全部加入連續(xù)相中。首先,單體進(jìn)行反應(yīng)生成預(yù)聚體,加入酸性催化劑后預(yù)聚體開始聚合,當(dāng)預(yù)聚體聚合尺寸逐步增大后,沉積在芯材物質(zhì)的表面而成囊。預(yù)聚體在連續(xù)相中是可溶的,而其聚合物在整個體系中是不可溶的,聚合反應(yīng)在分散相芯材上發(fā)生。 阿維菌素是一種以胃毒作用為主和兼有觸殺作用的生物殺螨、殺蟲、殺線蟲劑,具有低毒、高效、無公害、與其他農(nóng)藥使用無交互抗性以及不易產(chǎn)生抗藥性等特點(diǎn),因此被廣泛應(yīng)用于害蟲防治。但是,阿維菌素在使用過程中易受紫外線和微生物的影響而發(fā)生分解,影響藥效的發(fā)揮。將阿維菌索微囊化可以減少阿維菌索在使用中的降解,延長其藥效,減少資源浪費(fèi),降低用藥成本。本文對原位聚合法反應(yīng)過程中的處方和工藝進(jìn)行了研究,并制備出符合要求的阿維菌索緩釋微囊。 首先確定了高效液相色譜檢測條件：色譜柱,大連依利特Hypersil (4.6mm×200mm,5μm)；流動相,甲醇—水(90：10)；流速,0.7mL/min；檢測波長,245nm。建立了阿維菌素微囊的高效液相色譜檢測方法,確定了藥物含量的檢測方法,確定了釋放介質(zhì)的組成及釋放度的測定方法。 預(yù)聚體的制備實驗中,經(jīng)過對處方和工藝的單因素考察確定了大致的范圍,分別以囊材的生成量和微囊的外觀為評價指標(biāo),通過正交設(shè)計優(yōu)化了了預(yù)聚體制備的處方和工藝,得到最優(yōu)的條件為：脲醛分子比1：1.8,pH=8.5,在70℃水浴溫度下緩慢攪拌反應(yīng)75min。制備得到無色透明、性質(zhì)穩(wěn)定的粘稠預(yù)聚體溶液。 乳劑的制備實驗中,首先對油相組成和乳化劑進(jìn)行了篩選,確定溶解有阿維菌素的質(zhì)量比為3：4的甲苯和氯苯的混合溶劑為油相,質(zhì)量比為1：2的阿拉們膠和AE09為復(fù)合乳化劑。經(jīng)過對乳劑制備處方和工藝的單因素考察確定了大致的范圍。通過正交優(yōu)化實驗得到乳劑最優(yōu)的制備條件為：油水質(zhì)量比為13：100,乳化劑占油相質(zhì)量的30%,剪切攪拌轉(zhuǎn)速為4000rpm,攪拌時間為4min。制備得到粒徑分布均勻,性質(zhì)穩(wěn)定的白色乳劑。 微囊的制備實驗中,首先確定了乳劑和預(yù)聚體的質(zhì)量比為1：3,考察了酸化過程中的工藝與處方參數(shù),通過正交優(yōu)化設(shè)計得到最佳的酸化工藝為：酸化pH=2.5,加酸速度3mL/min,攪拌速度600rpm,室溫下酸化1.5h。并通過加入抗粘劑改善了微囊的粘連情況。對助懸劑的種類和用量進(jìn)行了篩選,確定1.0%的黃原膠作為微囊混懸液的助懸劑。 最終得到了外觀為均勻白色的微囊混懸液,經(jīng)測定微囊粒徑在1-12μm,跨距為1.604,藥物含量2.0±0.1%,包封率98.6%以上。于阿維菌素乳劑相比有顯著的緩釋作用,釋放度符合要求。
[Abstract]:In situ polymerization is a new method for preparing microcapsules. The soluble prepolymer and acid catalyst were added to the continuous phase with the core material as the dispersed phase. First, the monomer reacts to form the prepolymer, and the prepolymer begins to polymerize after adding the acid catalyst. When the size of the prepolymer increases gradually, the prepolymer is deposited on the surface of the core material to form a capsule. The prepolymer is soluble in the continuous phase, while the polymer is insoluble in the whole system, and the polymerization takes place on the core of the dispersed phase. Abamectin is a kind of biological mite killing, insecticidal and nematicidal agent, which is mainly caused by stomach toxicity and has contact effect. It has the characteristics of low toxicity, high efficiency, no pollution, no cross resistance with other pesticides, and is not easy to produce resistance to insecticides. Therefore, it is widely used in pest control. However, abamectin is easy to decompose under the influence of UV and microorganism, which affects the effect of Avermectin. Microencapsulation of avermectin can reduce the degradation of Avernoid in use, prolong its efficacy, reduce the waste of resources and reduce the cost of medication. In this paper, the formulation and process of in situ polymerization reaction were studied, and Avermectin sustained-release microcapsules were prepared. The detection conditions were determined as follows: column, 4.6mm 脳 200mm-1 5 渭 m); mobile phase, methanol-water (90:10), flow rate, 0.7 mL / min, detection wavelength, 245 nm. A high performance liquid chromatography (HPLC) method for the determination of abamectin microcapsules was established. In the preparation experiment of prepolymer, the formulation and process of prepolymer were optimized by orthogonal design, taking the quantity of capsule and the appearance of microcapsule as evaluation indexes. The optimum conditions are as follows: the molar ratio of urea-formaldehyde is 1: 1.8g, pH = 8.5, stirring slowly at 70 鈩，

本文編號：2292903