农药-LDHs纳米杂化物/农药微乳液复合体系研究
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摘要
本文的主要任务是研究农药-层状双金属氢氧化物(LDHs)纳米杂化物/农药微乳液复合体系的制备及性能,其总体目标是探索开发一类新型的农药剂型。
我国是世界上第二大农药生产国,年产值近200亿元,但与发达国家相比,长期存在剂型结构不合理,制剂质量差等问题。目前,我国的农药制剂仍以传统的乳油、悬浮剂和可湿性粉剂等为主,约占到制剂总量的80%。随着人们环保意识的增强和对药效期求的提高,逐渐认识到这些传统剂型存在生物利用率低、环境污染严重等问题,开发新型农药剂型已成为农药行业的首要任务之一。
农药-层状双金属氢氧化物(LDHs)纳米杂化物控释剂型和微乳液剂型是近年来开发的具有发展潜力的新剂型。
层状双金属氢氧化物(Layered Double Hydroxides,LDHs)是具有层状结构无机纳米材料,层片带结构正电荷,层间存在可交换的阴离子,农药分子可插入LDHs的层间(俗称通道)形成农药-LDHs纳米杂化物,具有良好的农药控释作用。但目前,国际上对农药-LDHs纳米杂化物控释剂型的研究还属初期阶段,没有成型产品面市,因为还有诸多问题需要研究解决,如分散性、悬浮性和粘附性有待于改善。
微乳剂是一种新兴的农药剂型,因其具有稳定性高、粘附力强、液滴微细而药效高等优点受到人们青睐。但微乳剂型也存在一些问题,主要是:药物选择性大,对一些药物的载药量太低;无控释效果,药效期短。
鉴于农药-LDHs纳米杂化物控释剂型和微乳液剂型各自存在的优点和不足,本研究拟将两个剂型相结合,保留各自的优点,克服各自的不足,开发一个新剂型,即农药-LDHs纳米杂化物/农药微乳液复合体系。
为实现以上目标,本文主要开展了以下研究工作:(1)LDHs及农药-LDHs纳米杂化物的制备及表征;(2)农药微乳液的制备及性能;(3)农药-LDHs纳米杂化物/农药微乳液复合体系的制备及作为农药制剂的性能评价。期望这些工作为农药新剂型的开发奠定基础和提供新思路。
本文主要获得以下结论:
1.采用共沉淀法分别制备了Mg-Al、Ni-Fe和Mg-Al-Fe型LDHs;Ni-Fe和Mg-Al-Fe型LDHs经高温煅烧可获得结构完整的尖晶石铁氧体相。
2.利用VSM技术对Ni-Fe和Mg-Al-Fe型LDHs及其煅烧产物进行了磁性研究。结果表明,Ni-Fe和Mg-Al-Fe型LDHs本身及其煅烧产物在常温下均呈现顺磁性,其煅烧产物均呈现超顺磁性;同类LDH中其煅烧产物的磁性大小与Fe~(3+)含量成正比而与LDH的晶体结构无关,Ni-Fe LDHs及其煅烧产物的磁性强于Mg-Al-Fe LDHs及其煅烧产物,。
3.发现了两个无表面活性剂微乳液(SFME)体系:呋喃甲醛/DMF/水和呋喃甲醛/乙醇/水体系。和传统微乳液一样,SFME也具有W/O、BC和O/W三个类型。温度和电解质对呋喃甲醛/DMF/水和呋喃甲醛/乙醇/水体系的相形为基本无影响。
4.呋喃甲醛/DMF/水和呋喃甲醛/乙醇/水两个SFME体系均具有很高的稳定性,常温储藏24个月、50℃热贮1周、-10℃冷冻-室温融化三个冻融循环和100g离心力下离心15分钟均未破坏其稳定性。
5.采用二次组装法制备了阿维菌素-LDHs纳米杂化物,具有明显的农药缓释效果,证明是有潜力的农药控释新剂型。
6.制备了阿维菌素SFME体系,具有良好的稳定性,证明SFME可用于农药微乳制剂。
7.制备了阿维菌素-LDHs纳米杂化物/阿维菌素微乳液复合体系,载药量较微乳剂明显提高,稳定性符合农药制剂要求,有望成为一类新型的农药制剂。
主要创新点:
1.发现了两个SFME体系:呋喃甲醛/DMF/水和呋喃甲醛/乙醇/水体系。和传统微乳液一样,SFME也具有W/O、BC和O/W三个类型。
2.采用二次组装法制备了阿维菌素-LDHs纳米杂化物,具有明显的农药缓释效果,证明是有潜力的农药控释新剂型。
3.制备了阿维菌素-LDHs纳米杂化物/阿维菌素微乳液复合体系,载药量较微乳剂明显提高,稳定性符合农药制剂要求,有望成为一类新型的农药制剂。
This paper aims at the preparation and properties of the pesticide-LDHs nanohybrid/pesticide-microemulsion, plan to develop a new kind of pesticide formulation.
Nowadays in china, the second biggest country of pesticide producing, preparations forms are mainly powder, oil concentrate and suspension concentrate, which are irrational and large application. Pesticide as brought many ignorant effects such as air pollutions, environmental destroy, food safety and so on, which has baffled agricultural sustainable development. Now the hit research trends of pesticide forms in the world are water-based, controlled release and multifunctional. Microemulsion has become one of the most popular research topics in the last decades because of its special advantages, such as efficient, environment-friendly, high stability.
Layered double hydroxides (LDHs), also called Hydrotalcite-like compounds (HTlc), consisting of divalent and trivalent metal ions and with the same layered crystal structure as Hydrotalcite, are a class of layered materials which has been paid a great of attention in recent years. The interlayer region of LDHs may be considered as a microvessle, some pesticide and drug molecules may be intercalated into the gallery of LDHs to form pesticide/drug-LDHs nanohybrids. The nanohybrids may evidently inhibit the release of molecules in the interlayer because of the hydrogen bond, van deel waals force and steric hindrance in LDHs gallery. LDHs can be potentially used in pesticide/drug delivery and controlled-release. But rare work has been done on pesticide-LDHs nanohybrid both in home and aboard. Many problems needed to be solve eagerly, such as dispersibility, suspension property, adhesive capacity and so on.
Microemulsion is a new type of pesticide delivery system. It has been widely researched in the last decade because the high stability, adherence and efficiency. The disadvantage of microemulsion is: (1) high pesticide selectivity; (2) low pesticide content; (3) difficult to control the release process.
In order to cover the shortage of the two formulations, this paper brings forward a new direction that the research of the LDH-SFME pesticide delivery compound system, which is a complementary of advantages of the two formulations.
Many works have been done to prepare and character the compound system and verify the feasibility of this direction. Primary works are: (1) preparation and characterization of LDHs and pesticide-LDHs nanohybrid; (2) Preparation and performance study of the pesticide microemulsion, especially the surfactant-free microemulsions (SFMEs); (3) Preparation of pesticide-LDHs/SFME system and its performance analysis as a pesticide formulation. Target to provide a new direction and foundation of novel pesticide formulations.
Primary conclusion:
1. Mg-Al, Ni-Fe and Mg-Al-Fe-LDHs were synthesised by coprecipitation method. Ferrite spinels with well crystal structure can obtained by calcination of Ni-Fe and Mg-Al-Fe-LDHs at a relative low temperature of 700℃.
2. The magnetic properties of Ni-Fe, Mg-Al-Fe-LDHs and their calcinates were studied in detail using a vibrating sample magnetometer(VSM). The Ni-Fe and Mg-Al-Fe-LDH show paramagnetism at normal temperature, the calcined samples of LDHs show super-paramagnetism. The magnetization increases with the higher Fe~(3+) content and is independent of the crystal structure of LDHs. Magnetization of the calcinates of Ni-Fe-LDHs is higher than the Mg-Al-Fe-LDHs.
3. Two novel SFME systems were found for the first time, that is furaldehyde/DMF/water and furaldehyde/ethanol/water system. Similar to the traditional microemulsion, SFME has three types of water in oil(W/O), bicontinuous(BC) and oil in water(O/W) microstructure. The phase behavior of the SFME system is independent of the temperature and salt concentration.
4. The stability of SFME system is excellent. The stability was examined by the following processes, respectively: (1) heat-storage at 80°C for one week; (2) cold-storage at -10℃for week; (3) freeze (-10℃)-thaw (40℃) cycle for 3 times; and (4) centrifugalized under 100 g for 15 min; (5) storage at room temperature for 24 months. It was found that their stability was not destroyed to the slightest degree and samples remained transparent.
5. Avermectin-LDHs(AM-LDHs) nanohybrid were prepared by re-assemble method, the pesticide released behavior is a slow-release process, providing that the LDHs is a novel pesticide slow-release formulation and the potential use as a controlled-release formulation is feasible.
6. Avermectin-SFME(AM-SFME) system was prepared and its stability is as good as the SFME system itself. Using SFME as a pesticide delivery system is practicable.
7. AM-LDHs/SFME compound system was prepared and characterized. The avermectin content is much higher than the AM-SFME system. The stability of the compound system satisfies the requirement as a pesticide formulation, its application as a pesticide delivery system is practicable.
Primary innovations:
1. Two novel SFME systems are found fo the first time consisting of furaldehyde/DMF/water and furaldehyde/ethanol/water. Similar to the traditional microemulsion, SFME also has three microstructures: water in oil(W/O), bicontinuous(BC) and oil in water(O/W).
2. Avermectin-LDHs(AM-LDHs) nanohybrid were prepared by re-assemble method, the pesticide released behavior is a slow-release process, providing that the LDHs is a novel pesticide slow-release formulation and the potential use as a controlled-release formulation is feasible.
3. AM-LDHs/SFME compound system was prepared as a example. The avermectin content is much higher than the AM-SFME system. The stability of the compound system satisfies the requirement as a pesticide formulation, its application as a pesticide delivery system is practicable.
我国是世界上第二大农药生产国,年产值近200亿元,但与发达国家相比,长期存在剂型结构不合理,制剂质量差等问题。目前,我国的农药制剂仍以传统的乳油、悬浮剂和可湿性粉剂等为主,约占到制剂总量的80%。随着人们环保意识的增强和对药效期求的提高,逐渐认识到这些传统剂型存在生物利用率低、环境污染严重等问题,开发新型农药剂型已成为农药行业的首要任务之一。
农药-层状双金属氢氧化物(LDHs)纳米杂化物控释剂型和微乳液剂型是近年来开发的具有发展潜力的新剂型。
层状双金属氢氧化物(Layered Double Hydroxides,LDHs)是具有层状结构无机纳米材料,层片带结构正电荷,层间存在可交换的阴离子,农药分子可插入LDHs的层间(俗称通道)形成农药-LDHs纳米杂化物,具有良好的农药控释作用。但目前,国际上对农药-LDHs纳米杂化物控释剂型的研究还属初期阶段,没有成型产品面市,因为还有诸多问题需要研究解决,如分散性、悬浮性和粘附性有待于改善。
微乳剂是一种新兴的农药剂型,因其具有稳定性高、粘附力强、液滴微细而药效高等优点受到人们青睐。但微乳剂型也存在一些问题,主要是:药物选择性大,对一些药物的载药量太低;无控释效果,药效期短。
鉴于农药-LDHs纳米杂化物控释剂型和微乳液剂型各自存在的优点和不足,本研究拟将两个剂型相结合,保留各自的优点,克服各自的不足,开发一个新剂型,即农药-LDHs纳米杂化物/农药微乳液复合体系。
为实现以上目标,本文主要开展了以下研究工作:(1)LDHs及农药-LDHs纳米杂化物的制备及表征;(2)农药微乳液的制备及性能;(3)农药-LDHs纳米杂化物/农药微乳液复合体系的制备及作为农药制剂的性能评价。期望这些工作为农药新剂型的开发奠定基础和提供新思路。
本文主要获得以下结论:
1.采用共沉淀法分别制备了Mg-Al、Ni-Fe和Mg-Al-Fe型LDHs;Ni-Fe和Mg-Al-Fe型LDHs经高温煅烧可获得结构完整的尖晶石铁氧体相。
2.利用VSM技术对Ni-Fe和Mg-Al-Fe型LDHs及其煅烧产物进行了磁性研究。结果表明,Ni-Fe和Mg-Al-Fe型LDHs本身及其煅烧产物在常温下均呈现顺磁性,其煅烧产物均呈现超顺磁性;同类LDH中其煅烧产物的磁性大小与Fe~(3+)含量成正比而与LDH的晶体结构无关,Ni-Fe LDHs及其煅烧产物的磁性强于Mg-Al-Fe LDHs及其煅烧产物,。
3.发现了两个无表面活性剂微乳液(SFME)体系:呋喃甲醛/DMF/水和呋喃甲醛/乙醇/水体系。和传统微乳液一样,SFME也具有W/O、BC和O/W三个类型。温度和电解质对呋喃甲醛/DMF/水和呋喃甲醛/乙醇/水体系的相形为基本无影响。
4.呋喃甲醛/DMF/水和呋喃甲醛/乙醇/水两个SFME体系均具有很高的稳定性,常温储藏24个月、50℃热贮1周、-10℃冷冻-室温融化三个冻融循环和100g离心力下离心15分钟均未破坏其稳定性。
5.采用二次组装法制备了阿维菌素-LDHs纳米杂化物,具有明显的农药缓释效果,证明是有潜力的农药控释新剂型。
6.制备了阿维菌素SFME体系,具有良好的稳定性,证明SFME可用于农药微乳制剂。
7.制备了阿维菌素-LDHs纳米杂化物/阿维菌素微乳液复合体系,载药量较微乳剂明显提高,稳定性符合农药制剂要求,有望成为一类新型的农药制剂。
主要创新点:
1.发现了两个SFME体系:呋喃甲醛/DMF/水和呋喃甲醛/乙醇/水体系。和传统微乳液一样,SFME也具有W/O、BC和O/W三个类型。
2.采用二次组装法制备了阿维菌素-LDHs纳米杂化物,具有明显的农药缓释效果,证明是有潜力的农药控释新剂型。
3.制备了阿维菌素-LDHs纳米杂化物/阿维菌素微乳液复合体系,载药量较微乳剂明显提高,稳定性符合农药制剂要求,有望成为一类新型的农药制剂。
This paper aims at the preparation and properties of the pesticide-LDHs nanohybrid/pesticide-microemulsion, plan to develop a new kind of pesticide formulation.
Nowadays in china, the second biggest country of pesticide producing, preparations forms are mainly powder, oil concentrate and suspension concentrate, which are irrational and large application. Pesticide as brought many ignorant effects such as air pollutions, environmental destroy, food safety and so on, which has baffled agricultural sustainable development. Now the hit research trends of pesticide forms in the world are water-based, controlled release and multifunctional. Microemulsion has become one of the most popular research topics in the last decades because of its special advantages, such as efficient, environment-friendly, high stability.
Layered double hydroxides (LDHs), also called Hydrotalcite-like compounds (HTlc), consisting of divalent and trivalent metal ions and with the same layered crystal structure as Hydrotalcite, are a class of layered materials which has been paid a great of attention in recent years. The interlayer region of LDHs may be considered as a microvessle, some pesticide and drug molecules may be intercalated into the gallery of LDHs to form pesticide/drug-LDHs nanohybrids. The nanohybrids may evidently inhibit the release of molecules in the interlayer because of the hydrogen bond, van deel waals force and steric hindrance in LDHs gallery. LDHs can be potentially used in pesticide/drug delivery and controlled-release. But rare work has been done on pesticide-LDHs nanohybrid both in home and aboard. Many problems needed to be solve eagerly, such as dispersibility, suspension property, adhesive capacity and so on.
Microemulsion is a new type of pesticide delivery system. It has been widely researched in the last decade because the high stability, adherence and efficiency. The disadvantage of microemulsion is: (1) high pesticide selectivity; (2) low pesticide content; (3) difficult to control the release process.
In order to cover the shortage of the two formulations, this paper brings forward a new direction that the research of the LDH-SFME pesticide delivery compound system, which is a complementary of advantages of the two formulations.
Many works have been done to prepare and character the compound system and verify the feasibility of this direction. Primary works are: (1) preparation and characterization of LDHs and pesticide-LDHs nanohybrid; (2) Preparation and performance study of the pesticide microemulsion, especially the surfactant-free microemulsions (SFMEs); (3) Preparation of pesticide-LDHs/SFME system and its performance analysis as a pesticide formulation. Target to provide a new direction and foundation of novel pesticide formulations.
Primary conclusion:
1. Mg-Al, Ni-Fe and Mg-Al-Fe-LDHs were synthesised by coprecipitation method. Ferrite spinels with well crystal structure can obtained by calcination of Ni-Fe and Mg-Al-Fe-LDHs at a relative low temperature of 700℃.
2. The magnetic properties of Ni-Fe, Mg-Al-Fe-LDHs and their calcinates were studied in detail using a vibrating sample magnetometer(VSM). The Ni-Fe and Mg-Al-Fe-LDH show paramagnetism at normal temperature, the calcined samples of LDHs show super-paramagnetism. The magnetization increases with the higher Fe~(3+) content and is independent of the crystal structure of LDHs. Magnetization of the calcinates of Ni-Fe-LDHs is higher than the Mg-Al-Fe-LDHs.
3. Two novel SFME systems were found for the first time, that is furaldehyde/DMF/water and furaldehyde/ethanol/water system. Similar to the traditional microemulsion, SFME has three types of water in oil(W/O), bicontinuous(BC) and oil in water(O/W) microstructure. The phase behavior of the SFME system is independent of the temperature and salt concentration.
4. The stability of SFME system is excellent. The stability was examined by the following processes, respectively: (1) heat-storage at 80°C for one week; (2) cold-storage at -10℃for week; (3) freeze (-10℃)-thaw (40℃) cycle for 3 times; and (4) centrifugalized under 100 g for 15 min; (5) storage at room temperature for 24 months. It was found that their stability was not destroyed to the slightest degree and samples remained transparent.
5. Avermectin-LDHs(AM-LDHs) nanohybrid were prepared by re-assemble method, the pesticide released behavior is a slow-release process, providing that the LDHs is a novel pesticide slow-release formulation and the potential use as a controlled-release formulation is feasible.
6. Avermectin-SFME(AM-SFME) system was prepared and its stability is as good as the SFME system itself. Using SFME as a pesticide delivery system is practicable.
7. AM-LDHs/SFME compound system was prepared and characterized. The avermectin content is much higher than the AM-SFME system. The stability of the compound system satisfies the requirement as a pesticide formulation, its application as a pesticide delivery system is practicable.
Primary innovations:
1. Two novel SFME systems are found fo the first time consisting of furaldehyde/DMF/water and furaldehyde/ethanol/water. Similar to the traditional microemulsion, SFME also has three microstructures: water in oil(W/O), bicontinuous(BC) and oil in water(O/W).
2. Avermectin-LDHs(AM-LDHs) nanohybrid were prepared by re-assemble method, the pesticide released behavior is a slow-release process, providing that the LDHs is a novel pesticide slow-release formulation and the potential use as a controlled-release formulation is feasible.
3. AM-LDHs/SFME compound system was prepared as a example. The avermectin content is much higher than the AM-SFME system. The stability of the compound system satisfies the requirement as a pesticide formulation, its application as a pesticide delivery system is practicable.
引文
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