CN101686664A - 用于植物保护的活性成分组合物 - Google Patents
用于植物保护的活性成分组合物 Download PDFInfo
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- CN101686664A CN101686664A CN200880021996A CN200880021996A CN101686664A CN 101686664 A CN101686664 A CN 101686664A CN 200880021996 A CN200880021996 A CN 200880021996A CN 200880021996 A CN200880021996 A CN 200880021996A CN 101686664 A CN101686664 A CN 101686664A
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Abstract
本发明涉及一种呈细碎的含活性物质颗粒形式的两于植物保护的新活性成分组合物,该组合物包含:a)至少一种植物的活性保护剂;b)至少一种不溶于水且可通过酶促水解降解的聚合物P,其量基于含活性物质颗粒的组分的总量为至少20重量%,和c)至少一种水解酶(EC 3),其中至少90重量%的活性成分组合物的含活性物质颗粒的直径不超过500μm(D90-值)且其中组分a)、b)和c)占活性物质颗粒的至少30重量%。本发明还涉及一种制备它们的方法以及活性成分组合物在处理植物、土壤和种子中的用途。
Description
本发明涉及用于植物保护的,呈细颗粒的含活性物质颗粒形式的新的活性物质组合物,一种制备它们的方法,以及活性物质组合物在处理植物、土壤和种子中的用途。
通过施用合适的植物保护产品保护有用的植物或作物植物防止对植物有害的生物体侵袭,控制调节有用植物的生长,以及对抗有害植物是增加产量,以及因此保护基于植物的食品的生产的重要手段。
施用用于对抗有害生物体的常规植物保护产品经常必然伴有缺点。因此,待对抗的生物体可能产生抗性,当长时间施用,或不适当施用时,尤其如此。此外,长期或不适当施用植物保护产品可能导致环境问题或伤害使用者。这就是企图找到使得控制施用并因此降低植物保护产品的施用率成为可能的植物保护产品的使用形式的原因。
许多植物,尤其是作物植物在萌发和发芽之前或过程中对植物病原性真菌或动物害虫侵袭高度敏感。这首先归因于植物本身尺寸小,这使得植物难以抵偿损害。另一方面,植物的自然防御机制在其早期生长阶段通常还未发育。因此,在萌发之前或过程中保护植物是减少植物损害的重要手段。
在植物的早期生长阶段,用于对抗对植物有害的生物体的植物保护剂的常规施用通常是不成功的。首先,较高施用率可能损害植物本身。然而,较低施用率通常不允许有效防治有害生物体。在某些方面,常规的种子处理是个办法。此处,种子在种植之前或过程中用合适的活性物质处理,该活性物质意欲保护植物在萌发或发芽之前或过程中防止有害生物体侵袭。常规种子处理中的问题为种植种子以及萌发和发芽段通常相隔一段时间。在该期间,活性物质可能由于环境因素,例如由于雨而被滤掉,以至于低施用率不再保证足够的保护。反之,较高施用率导致上述问题且额外构成了显著的消耗。常规种子处理中的其它问题为植物毒性的副作用和施用于种子的活性物质对植物生长的负面影响。另外,活性物质的受控制的,即延迟的释放应修正该问题或者至少减少这些问题。
因此,并不缺乏以允许控制释放活性物质的方式配制活性物质的尝试。
因此,WO 99/00013描述了用于控制释放植物保护剂的活性物质组合物,该组合物包含细颗粒状的活性物质颗粒,其中植物保护剂分布在聚合物基质中。通常而言,聚合物基质由一种不溶于水的聚合物和一种溶于水的聚合物组成。通常而言,活性物质由于含活性物质颗粒的分解而释放,其由颗粒的可溶于水的聚合物组分溶解而引发。虽然,活性物质的滤出可以该方式减少且获得活性物质的更均匀释放时,但是活性物质的释放极大地取决于土壤中的水分条件。
JP 2002/360665又公开了尺寸为数毫米的粗胶囊,该胶囊具有一个核和至少两个包围该核的涂层。外涂层具有至少一种外层或其下的层借助其降解的酶。这些胶囊可用作人工种子或用于给药。这类胶囊不适于处理土壤或种子。
因此,本发明基于的问题为提供适于处理种子或土壤且允许控制释放活性物质的活性物质组合物,该控制释放不取决于土壤的水分含量。
令人惊讶的是,该问题通过下文所述的活性物质组合物解决。
因此,本发明涉及一种呈细碎的含活性物质颗粒形式的活性物质组合物,该组合物包含:
a)至少一种植物保护剂;
b)至少一种不溶于水且可通过酶促水解降解的聚合物P,其量基于含活性物质颗粒的组分的总量为至少20重量%,经常至少30重量%,优选至少40重量%,尤其是至少45重量%,特别是至少50重量%,和
c)至少一种水解酶(EC 3),
其中至少90重量%的活性物质组合物的含活性物质颗粒的直径不超过500μm(D90-值),且其中组分a)、b)和c)占活性物质颗粒的至少30重量%,经常至少40重量%,尤其是至少50重量%,特别是至少60重量%。
在本发明的活性化合物组合物中,水解酶引起聚合物P的酶促降解,这导致了活性物质颗粒的崩解并因此导致了活性物质从颗粒中释放。
不像现有技术的细碎的聚合物包封的活性物质组合物那样,活性物质颗粒不仅仅由于水分而崩解,而且额外需要足够的温度,因为否则水解酶的活性就太低,不能引起聚合物P的有效降解。然而,当温度达到植物生长或种子开始萌发或发芽的范围时,水解酶通常存在足够活性。因此,本发明组合物确保活性物质在植物需要的时间点释放。因此,本发明活性物质组合物特别适于处理种子和土壤。
因此,本发明进一步涉及活性物质组合物在处理土壤和处理种子中的用途。本发明进一步涉及包含该活性物质组合物的种子。
本发明活性物质组合物还导致在植物处理中较好的耐受性和增加的效率。因此,本发明涉及活性物质组合物在植物处理中的用途。
本发明活性物质组合物包含至少一种可通过酶促水解而降解,但其本身不溶于水的聚合物P。不溶于水的聚合物应理解为指其中在25℃下,甚至在48小时后,5g样品在1升水中还没有完全溶解的那些聚合物。
通常而言,可通过酶促水解而降解的聚合物为作为可生物降解的聚合物而被熟练技术人员已知的那些聚合物,即符合DIN V 54900中规定的生物降解性定义的聚合物。
可生物降解通常指聚合物在合适且可检测的时间内崩解。通常而言,降解以水解进行;其主要由微生物如细菌、酵母、真菌和藻类的作用,或由包含在其中的水解酶引起。生物降解性例如可通过将聚合物与堆肥混合并将混合物储存特定时间而测定。根据ASTM D 5338、ASTM D 6400和DIN V 54900,使不含CO2的空气例如在堆肥处理过程中通过熟化堆肥,且使该堆肥经受规定的温度条件。这经由样品的净CO2释放量(在减去不含样品的堆肥的CO2释放量之后)与样品的最大CO2释放量(经由样品的碳含量计算)的比例定义生物降解性。通常而言,可生物降解的聚合物,尤其是可生物降解的聚酯在堆肥仅数天之后显示了显著的降解症状如真菌建群、撕裂和孔形成。这类聚合物是熟练技术人员已知的且可市购。
可通过酶促水解降解的聚合物P通常在聚合物骨架上具有多个可水解的官能团。通常它们呈酯基或酰胺基、脲基、氨基甲酸乙酯基或缩醛基的形式。作为替代,可通过酶促水解而降解的聚合物还可具有与聚合物骨架键接且赋予水解后聚合物增加的水溶性的可水解的官能团。
对于本发明组合物,可通过酶促水解而降解的聚合物P的分子量可在宽范围内变化,且通常为1000-1000000,经常5000-500000,特别是10000-2500000(数均)。
聚合物P优选具有大于40℃,例如40-180℃,尤其是60-160℃的熔点或玻璃化转变温度。
聚合物P优选在聚合物骨架上具有多个可水解的官能团,尤其是酯基。
在聚合物骨架上具有多个酯基的聚合物尤其应理解为指聚丙交酯、聚己内酯、聚丙交酯和聚C2-C4亚烷基二醇的嵌段共聚物、聚己内酯和聚C2-C4亚烷基二醇的嵌段共聚物以及下文所定义的共聚酯,所述共聚酯至少由脂族或脂环族二元羧酸或其成酯衍生物和至少一种脂族或脂环族二元醇组分和合适的话其它组分组成。
术语“聚丙交酯”应理解为指乳酸的缩聚物。合适的聚丙交酯描述在WO 97/41836、WO 96/18591、WO 94/05484、US 5,310,865、US 5,428,126、US 5,440,008、US 5,142,023、US 5,247,058、US 5,247,059、US 5,484,881、WO 98/09613、US 4,045,418、US 4,057,537和Adv.Mater.2000,12,1841-1846中。这些产品呈基于乳酸内酯(A)的聚合物的形式,(A)经由开环聚合转化为聚乳酸聚合物(B):
在式(B)中,聚合度n为1000-4000,优选1500-3500,特别优选1500-2000(数均)。取决于聚合度,这些产物的平均摩尔质量(数均)为71,000-284,000g/mol。合适的聚丙交酯例如可由Cargill Dow LLC(例如PLA聚合物4041D、PLA聚合物4040D、PLA聚合物4031D、PLA聚合物2000D或PLA聚合物1100)或Mitsui Chemicals(Lactea)获得。特别优选的式(B)聚合物的平均摩尔质量(数据)各自为118,000g/mol(Lactea)、212,000g/mol(PLA聚合物4041D)和223,000g/mol(PLA聚合物2000D)。
聚丙交酯和聚C2-C4亚烷基二醇,尤其是与聚乙二醇的二嵌段和三嵌段共聚物也是合适的。这些嵌段共聚物例如可由Aldrich(例如产品号659649)获得。它们可呈具有聚丙交酯嵌段和聚C2-C4氧化烯嵌段的聚合物的形式。这类嵌段共聚物例如可通过在聚C2-C4亚烷基二醇存在下乳酸的缩聚或通过乳酸内酯(A)的开环聚合而得到。
根据本发明适合的聚合物P尤其是聚己内酯。它们由熟练技术人员理解为指通过下文的式D描述的聚合物,其中n为聚合物中重复单元的数目,即聚合度。
在式(D)中,聚合度n为100-1000,优选500-1000(数均)。取决于聚合度,这些产物的数均分子量为10000g/mol-100000g/mol。特别优选的式(D)聚合物的平均摩尔质量(数均)为50000g/mol(CAPA 6500)、80000g/mol(CAPA 6800)和100000g/mol(CAPA FB 100)。
通常而言,聚己内酯通过ε-己内酯(化合物C)在催化剂存在下开环聚合而制备。
聚己内酯可由Solvay以CAPA聚合物,例如CAPA 6100、6250、6500或CAPA FB 100购得。
此外,合适的聚合物P为聚己内酯与聚C2-C4亚烷基二醇,尤其是与聚乙二醇(=聚氧化乙烯)的二嵌段和三嵌段共聚物,即具有至少一个式D的聚己内酯嵌段和至少一个聚亚烷基二醇嵌段的聚合物。例如类似于Macromolecules 2003,36,8825-8829及随后各页中所述方法,这类聚合物例如可通过使己内酯在聚亚烷基二醇存在下聚合而制备。
根据本发明适合的其它聚合物P尤其为包含至少一种脂族或脂环族二羧酸或一种其成酯衍生物和至少一种脂族或脂环族二元醇组分和合适的话其它组分的共聚酯。它们尤其呈由包含如下物质的共聚酯的形式:
A)包含如下物质的酸组分:
a1)30-100摩尔%的至少一种脂族或至少一种脂环族二元羧酸或其成酯衍生物或混合物,
a2)0-70摩尔%的至少一种芳族二元羧酸或其成酯衍生物或其混合物,和
a3)0-5摩尔%的具有至少两个羧基的含磺酸根的化合物,
其中组分a1)-a3)的摩尔百分数总共为100%,和
B)选自C2-C12链烷二醇、C5-C10环烷二醇及其混合物的二元醇组分,和需要的话
C)一种或多种除了A和B之外的可酯化组分作为组分C。
根据本发明适合的二元羧酸a1)通常具有2-10个碳原子,优选4-8个,尤其是6个碳原子。它们可为线性和支化。通常而言,用于本发明目的的脂环族二元羧酸为具有7-10个碳原子的那些,尤其是具有8个碳原子的那些。然而,原则上还可使用具有较大量碳原子,例如具有至多30个碳原子的二元羧酸。可提到的实例为:丙二酸、琥珀酸、戊二酸、2-甲基戊二酸、3-甲基戊二酸、己二酸、庚二酸、壬二酸、癸二酸、富马酸、2,2-二甲基戊二酸、辛二酸、1,3-环戊烷二甲酸、1,4-环己烷二甲酸、1,3-环己烷二甲酸、二甘醇酸、衣康酸、马来酸和2,5-降莰烷二甲酸。可同样使用的上述脂族或脂环族二元羧酸的成酯衍生物尤其为二C1-C6烷基酯,如二甲酯、二乙酯、二正丙酯、二异丙酯、二正丁酯、二异丁酯、二叔丁酯、二正戊酯、二异戊酯或二正己酯。同样可使用二元羧酸的酐。特别优选使用的物质为己二酸或琥珀酸,它们各自的成酯衍生物或其混合物。
可提到的芳族二元羧酸a2通常为具有8-12个碳原子的那些,优选具有8个碳原子的那些。可提到的实例为对苯二甲酸、间苯二甲酸、2,6-萘甲酸和1,5-萘二甲酸,以及其成酯衍生物。就此而言,尤其可提到二C1-C6烷基酯,例如二甲酯、二乙酯、二正丙酯、二异丙酯、二正丁酯、二异丁酯、二叔丁酯、二正戊酯、二异戊酯或二正己酯。二元羧酸a2的酐也是合适的成酯衍生物。然而,原则上也可使用具有较大量碳原子,例如至多20个碳原子的芳族二元羧酸a2。芳族二元羧酸或其成酯衍生物a2可单独使用或以它们的两种或更多种的混合物使用。特别优选使用对苯二甲酸或其成酯衍生物如对苯二甲酸二甲酯。
通常使用的含磺酸根的化合物为含磺酸根的二元羧酸或其成酯衍生物的碱金属或碱土金属盐,优选5-磺基间苯二甲酸或其混合物的碱金属盐,特别优选钠盐。
通常而言,二元醇B选自具有2-12个碳原子,优选4-8个或尤其是6个碳原子的支化或线性链烷二醇,或具有5-10个碳原子的环烷二醇。
合适的链烷二醇的实例为乙二醇、1,2-丙二醇、1,3-丙二醇、1,2-丁二醇、1,4-丁二醇、1,5-戊二醇、2,4-二甲基-2-乙基己烷-1,3-二醇、2,2-二甲基-1,3-丙二醇、2-乙基-2-丁基-1,3-丙二醇、2-乙基-2-异丁基-1,3-丙二醇、2,2,4-三甲基-1,6-己二醇,尤其是乙二醇、1,3-丙二醇、1,4-丁二醇和2,2-二甲基-1,3-丙二醇(新戊二醇);环戊二醇、1,4-环己二醇、1,2-环己烷二甲醇、1,3-环己烷二甲醇、1,4-环己烷二甲醇或2,2,4,4-四甲基-1,3-环丁二醇。也可使用不同链烷二醇的混合物。
取决于是否需要过量的酸或OH端基,可过量使用组分A或组分B。根据优选的实施方案,所用组分A和B的摩尔比例可为0.4∶1-1.5∶1,优选0.6∶1-1.1∶1。
除了组分A和B,聚酯可包含掺入的其它组分C和/或D。组分C包括:
c1)式I的二羟基化合物:
HO-[(A)-O]m-H (I)
其中A为C2-C4亚烷基单元,如1,2-乙烷二基、1,2-丙烷二基、1,3-丙烷二基或1,4-丁烷二基,且m为2-250的整数;
c2)式IIa或IIb的羟基羧酸:
其中p表示1-1500的整数,r表示1-4的整数,G为选自亚苯基、其中q为1-5的整数的-(CH2)q-、其中R为甲基或乙基的-C(R)H-和-C(R)HCH2的基团;
c3)氨基-C2-C12链烷醇、氨基-C5-C10环烷醇或它们的混合物;
c4)二氨基-C1-C8链烷烃;
c5)通式III的2,2′-双噁唑啉:
其中R1表示单键、其中z=2、3或4的(CH2)z-亚烷基,或亚苯基;
c6)氨基羧酸,选自天然氨基酸,可通过使具有4-6个碳原子的二元羧酸与具有4-10个碳原子的二胺缩聚而获得的分子量不超过18000g/mol的聚酰胺,式IVa和IVb的化合物:
其中s为1-1500的整数,t为1-4的整数,且T为选自亚苯基、其中u为1-12的整数的-(CH2)u-、其中R2为甲基或乙基的-C(R2)H-和-C(R2)HCH2,以及具有重复单元V的聚噁唑啉:
其中R3表示氢、C1-C6烷基、C5-C8环烷基、未被取代的苯基或由C1-C4烷基至多三取代的苯基,或表示四氢呋喃基;
c7)具有至少三个可酯化基团的化合物;
c8)异氰酸酯,和
c9)二乙烯基醚。
组分c1的实例为二甘醇、三甘醇、聚乙二醇、聚丙二醇和聚四氢呋喃(聚THF),特别优选二甘醇、三甘醇和聚乙二醇,其中也可使用它们的混合物或具有不同亚烷基单元A(参见式I)的化合物,如包含亚丙基单元的聚乙二醇(A=1,2-或1,3-丙烷二基)。后者例如可通过本身已知的方法首先使氧化乙烯,随后使氧化丙烯聚合而获得。特别优选基于具有不同变量A的聚亚烷基二醇的共聚物,其中氧化乙烯所形成单元(A=1,2-乙烷二基)占优势。聚乙二醇的分子量(数均Mn)通常选自250-8000,优选600-3000g/mol的范围。
根据一个优选实施方案,对制备共聚酯而言,例如可使用基于B和c1的摩尔量为15-98摩尔%,优选60-99.5摩尔%二元醇B和0.2-85摩尔%,优选0.5-30摩尔%二羟基化合物c1。
优选组分c2的实例为乙醇酸,D-、L-,、D,L-乳酸,6-羟基己酸,其环状衍生物如乙交酯(1,4-二噁烷-2,5-二酮)、D-,L-双丙交酯(3,6-二甲基-1,4-二噁烷-2,5-二酮),对羟基苯甲酸及其低聚物,或聚合物如3-聚羟基丁酸、聚羟基戊酸、聚丙交酯(例如可以(Cargill)获得)和3-聚羟基丁酸和聚羟基戊酸的混合物(其中后者可以得自Zeneca)。对制备共聚酯而言,特别优选它们的低分子量和环状衍生物。羟基羧酸或其低聚物和/或聚合物例如可以基于A和B的量以0.01-50重量%,优选0.1-40重量%的量使用。
优选组分c3为氨基-C2-C6链烷醇,如2-氨基乙醇、3-氨基丙醇、4-氨基丁醇、5-氨基戊醇、6-氨基己醇,以及氨基-C5-C6-环烷醇如氨基环戊醇和氨基环己醇,或它们的混合物。
优选组分c4为二氨基-C4-C6链烷烃,如1,4-二氨基丁烷、1,5-二氨基戊烷和1,6-二氨基己烷。
根据优选实施方案,将基于B的摩尔量为0.5-99.5摩尔%,优选0.5-50摩尔%的c3和基于B的摩尔量为0-50摩尔%,优选0-35摩尔%的c4用于制备共聚酯。
组分c5)的优选双噁唑啉III为其中R1表示单键,其中z=2、3或4的(CH2)z-亚烷基如亚甲基、乙烷-1,2-二基、丙烷-1,3-二基、丙烷-1,2-二基或亚苯基的那些。可作为特别优选的双噁唑啉提到的那些为2,2′-二(2-噁唑啉)、二(2-噁唑啉基)甲烷、1,2-二(2-噁唑啉基)乙烷、1,3-二(2-噁唑啉基)丙烷或1,4-二(2-噁唑啉基)丁烷、1,4-二(2-噁唑啉基)苯、1,2-二(2-噁唑啉基)苯或1,3-二(2-噁唑啉基)苯。通式III的双噁唑啉通常可通过Angew.Chem.Int.Edit.,Vol.11(1972),第287-288页的方法获得。
为制备聚酯,例如可使用在每种情况下基于组分B、c3、c4和c5的总摩尔量为70-98摩尔%的B,至多30摩尔%的c3,至多30摩尔%,例如0.5-30摩尔%的c4,以及至多30摩尔%,例如0.5-30摩尔%的c5。根据另一优选实施方案,可使用基于A和B的总重量为0.1-5重量%,优选0.2-4重量%的c5。
天然氨基羧酸可用作组分c6。它们包括缬氨酸、亮氨酸、异亮氨酸、苏氨酸、蛋氨酸、苯基丙氨酸、色氨酸、赖氨酸、丙氨酸、精氨酸、天冬氨酸、半胱氨酸、谷氨酸、甘氨酸、组胺酸、脯氨酸、丝氨酸、酪氨酸、天冬酰胺或谷氨酰胺。
优选的通式IVa和IVb的氨基羧酸为其中s为1-1000的整数,t为1-4,优选1或2的整数,且T选自亚苯基和其中u为1、5或12的-(CH2)u-的那些。
此外,c6也可为通式V的聚噁唑啉。然而,组分c6也可为不同氨基羧酸和/或聚噁唑啉的混合物。
根据优选实施方案,c6可以基于组分A和B的总量以0.01-50重量%,优选0.1-40重量%的量使用。
可任选用于制备聚酯的其它组分包括化合物c7,其包含至少三个可酯化基团。化合物c7优选包含3-10个能够形成酯键的官能团。特别优选的化合物c7在分子中具有3-6个该类官能团,尤其是3-6个羟基和/或羧基。可提到的实例为:酒石酸、柠檬酸、苹果酸;三羟甲基丙烷、三羟甲基乙烷;季戊四醇;聚醚三醇;甘油;苯均三酸;偏苯三酸及其酐;苯均四酸及其二酐,以及羟基间苯二甲酸。需要的话,化合物c7的用量通常基于组分A为0.01-15摩尔%,优选0.05-10摩尔%,特别优选0.1-4摩尔%。
可用作组分c8的物质为芳族或脂族二异氰酸酯。然而,也可使用具有较高官能度的异氰酸酯。芳族二异氰酸酯的实例为甲苯2,4-二异氰酸酯、甲苯2,6-二异氰酸酯、2,2′-二苯基甲烷二异氰酸酯、2,4′-二苯基甲烷二异氰酸酯、4,4′-二苯基甲烷二异氰酸酯、萘1,5-二异氰酸酯或苯二亚甲基二异氰酸酯。脂族二异氰酸酯的实例主要为具有2-20个碳原子,优选3-12个碳原子的线性或支化的亚烷基二异氰酸酯或亚环烷基二异氰酸酯,例如1,6-六亚甲基二异氰酸酯,异佛尔酮二异氰酸酯或亚甲基二(4-异氰酸根合环己烷)。此外,适合作为组分c8的物质为三(4-异氰酸根合苯基)甲烷和上述二异氰酸酯的氰脲酸酯、缩脲二酮和缩二脲。
需要的话,组分c8的用量通常为基于A和B的总摩尔量为0.01-5摩尔%,优选0.05-4摩尔%,特别优选0.1-4摩尔%。
可使用的二乙烯基醚c9通常是所有常规且可市购的二乙烯基醚。优选使用如下:1,4-丁二醇二乙烯基醚、1,6-己二醇二乙烯基醚或1,4-环己烷二甲醇二乙烯基醚或它们的混合物。二乙烯基醚的用量优选基于A和B的总重量为0.01-5重量%,尤其是0.2-4重量%。
共聚酯例如由WO96/15173和WO 04/67632已知,或可通过本身已知的方法制备。
优选的共聚酯的数均分子量(Mn)为1000-100000g/mol,尤其是9000-75000g/mol,优选30000-80000g/mol。它们优选具有60-170℃,尤其是60-150℃的熔点。
上述共聚酯可以任何所需比例具有羟基和/或羧基端基。上述共聚酯也可以是端基改性的。因此,OH端基例如可通过与邻苯二甲酸、邻苯二甲酸酐、偏苯三酸、偏苯三酸酐、苯均四酸或苯均四酸酐反应而酸改性。
在本发明的一个实施方案中,可使用的聚合物P也可为各种包含酯基的聚合物P的混合物,例如上述共聚酯与聚己内酯或聚丙交酯的混合物,以及包含酯基的聚合物P与其它生物聚合物如淀粉或与改性的可生物降解的生物聚合物如改性淀粉、纤维素酯(如纤维素乙酸酯、纤维素乙酸丁酸酯)或可生物降解的人造聚合物如聚丙交酯(例如可以(Cargill)获得)的混合物。
在本发明的一个优选实施方案中,聚合物P选自聚丙交酯、聚己内酯、聚丙交酯与聚C2-C4亚烷基二醇,特别是与聚乙二醇的嵌段共聚物,以及聚己内酯与聚C2-C4亚烷基二醇,特别是与聚乙二醇的嵌段共聚物。
特别优选的聚合物P为聚己内酯,尤其是数均分子量为50000-100000g/mol的那些,特别优选数均分子量为80000-100000g/mol的那些。特别优选的聚合物P还有聚己内酯与聚C2-C4亚烷基二醇,特别是与聚乙二醇的嵌段共聚物,尤其是数均分子量为50000-100000g/mol的那些,特别优选数均分子量为80000-100000g/mol的那些。
通常选择聚合物P的量,以使得聚合物颗粒的崩解仅通过聚合物的酶促降解,即在曝露于水分时在所需温度之上而实现。因此,聚合物P的量通常基于形成活性物质颗粒的组分的总质量为至少20重量%,经常至少30重量%,优选至少40重量%,尤其是至少45重量%,特别优选至少50重量%。聚合物P含量的上限自然受必须存在的其它组分限制,且因此基于形成活性物质颗粒的组分的总量不超过99重量%,尤其是95重量%,特别是94重量%。通常而言,聚合物P含量在每种情况下基于含活性物质颗粒的组分的总量为20-99重量%,经常30-95重量%,优选40-95重量%,尤其是45-94重量%,特别是50-90重量%,或50-89重量%或50-80重量%。
在本申请中,术语“总量”对应于活性物质组合物的组分的总重量,其涉及活性物质组合物中的组分。术语“活性物质颗粒的组分”对应于术语“活性物质组合物的组分”。
根据本发明,活性物质组合物包含至少一种植物保护剂。在本发明上下文中,术语“植物保护剂”应在宽意义上理解且不仅包括保护植物防止有害生物体侵袭的物质,破坏对植物有害的生物体或防止它们发育的物质,以及调节有用植物生长,即促进或减少生长的物质,其包括用于促进植物健康的物质。植物保护剂例如包括:
-杀虫剂、杀螨剂和杀线虫剂,即破坏对植物有害的节肢动物或线虫的物质或以使得有用植物的侵袭被有效防止或减少这些有害生物体侵袭植物的方式降低其发育的活性物质;
-杀真菌剂,即破坏植物病原性真菌或防止其生长或减少这类植物病原性真菌侵袭有用植物的活性物质;
-除草剂,即破坏有害植物或减少或防止其生长的活性物质;
-生长调节剂,即促进或减少植物生长的活性物质;
-安全剂,即减少或防止植物毒性对有用植物的影响的活性物质,该影响由上述物质引起;和
-肥料。
植物保护剂优选为有机植物保护剂,尤其是分子量为150-500道尔顿的低分子量有机植物保护剂。
植物保护剂优选在室温下为固体或非挥发性油,即其蒸气压在25℃下小于0.1毫巴。
合适的植物保护剂的实例列在下文中。具有杀虫、杀螨和/或杀线虫活性的活性物质的实例在组A.1-15中提到:
A.1.有机(硫代)磷酸酯类:高灭磷(acephate)、唑啶磷(azamethiphos)、谷硫磷(azinphos-methyl)、毒死蜱(chlorpyrifos)、甲基毒死蜱(chlorpyriphos-methyl)、毒虫畏(chlorfenvinphos)、二嗪农(diazinon)、敌敌畏(dichlorvos)、百治磷(dicrotophos)、乐果(dimethoate)、乙拌磷(disulfoton)、乙硫磷(ethion)、杀螟松(fenitrothion)、倍硫磷(fenthion)、异噁唑磷(isoxathion)、马拉硫磷(malathion)、甲胺磷(methamidophos)、杀扑磷(methidathion)、甲基一六零五(methyl parathion)、速灭磷(mevinphos)、久效磷(monocrotophos)、砜吸磷(oxydemetonmethyl)、对氧磷(paraoxon)、一六零五(parathion)、稻丰散(phenthoate)、伏杀磷(phosalone)、亚胺硫磷(phosmet)、磷胺(phosphamidon)、甲拌磷(phorate)、辛硫磷(phoxim)、虫螨磷(pirimiphosmethyl)、丙溴磷(profenofos)、丙硫磷(prothiofos)、乙丙硫磷(sulprofos)、杀虫畏(tetrachlorvinphos)、特丁磷(terbufos)、三唑磷(triazophos)、敌百虫(trichlorfon);
A.2.氨基甲酸酯类:棉铃威(alanycarb)、涕灭威(aldicarb)、噁虫威(bendiocarb)、丙硫克百威(benfuracarb)、甲奈威(carbaryl)、虫螨威(carbofuran)、丁硫克百威(carbosulfan)、双氧威(fenoxycarb)、呋线威(furathiocarb)、灭虫威(methiocarb)、灭多虫(methomyl)、甲氨叉威(oxamyl)、抗蚜威(pirimicarb)、残杀威(propoxur)、硫双威(thiodicarb)、唑蚜威(triazamate);
A.3.合成除虫菊酯类:丙烯除虫菊(allethrin)、氟氯菊酯(bifenthrin)、氟氯氰菊酯(cyfluthrin)、(RS)氯氟氰菊酯(cyhalothrin)、苯醚氰菊酯(cyphenothrin)、氯氰菊酯(cypermethrin)、甲体氯氰菊酯(alpha-cypermethrin)、乙体氯氰菊酯(beta-cypermethrin)、己体氯氰菊酯(zeta-cypermethrin)、溴氰菊酯(deltamethrin)、高氰戊菊酯(esfenvalerate)、醚菊酯(ethofenprox)、甲氰菊酯(fenpropathrin)、杀灭菊酯(fenvalerate)、咪炔菊酯(imiprothrin)、λ-氯氟氰菊酯(lambda-cyhalothrin)、γ-氯氟氰菊酯(gamma-cyhalothrin)、氯菊酯(permethrin)、炔酮菊酯(prallethrin)、除虫菊(pyrethrin)I和II、灭虫菊(resmethrin)、灭虫硅醚(silafluofen)、氟胺氰菊酯(tau-fluvalinate)、七氟菊酯(tefluthrin)、胺菊酯(tetramethrin)、四溴菊酯(tralomethrin)、四氟菊酯(transfluthrin)、profluthrin和dimefluthrin;
A.4.生长调节剂:a)几丁质合成抑制剂:苯甲酰脲类:定虫隆(chlorfluazuron)、氟脲杀(diflubenzuron)、氟螨脲(flucycloxuron)、氟虫脲(flufenoxuron)、氟铃脲(hexaflumuron)、氟丙氧脲(lufenuron)、双苯氟脲(novaluron)、伏虫隆(teflubenzuron)、杀虫隆(triflumuron);噻嗪酮(buprofezin)、噁茂醚(diofenolan)、噻螨酮(hexythiazox)、特苯噁唑(etoxazole)、四螨嗪(clofentazine);b)蜕皮激素拮抗剂:特丁苯酰肼(halofenozide)、甲氧苯酰肼(methoxyfenozide)、双苯酰肼(tebufenozide)、艾扎丁(azadirachtin);c)保幼激素类似物:蚊蝇醚(pyriproxyfen)、蒙五一五(methoprene)、双氧威(fenoxycarb);d)类脂生物合成抑制剂:螺螨酯(spirodiclofen)、螺甲螨酯(spiromesifen)、spirothtramate;
A.5.烟碱受体激动剂/拮抗剂化合物:噻虫胺(clothianidin)、呋虫胺(dinotefuran)、吡虫啉(imidacloprid)、噻虫嗪(thiamethoxam)、硝胺烯啶(nitenpyram)、吡虫清(acetamiprid)、噻虫啉(thiacloprid)、式Г1的噻唑化合物:
A.6.GABA拮抗剂化合物:acetoprole、硫丹(endosulfan)、乙虫清(ethiprole)、锐劲特(fipronil)、氟吡唑虫(vaniliprole)、pyrafluprole、pyriprole、式Г2的苯基吡唑化合物:
A.7.大环内酯杀虫剂:齐墩螨素(abamectin)、甲氨基阿维菌素(emamectin)、米尔螨素(milbemectin)、lepimectin、艾克敌105(spinosad)、式Γ3化合物(CAS No.187166-40-1):
A.8.METI I化合物:芬杀螨(fenazaquin)、哒螨酮(pyridaben)、吡螨胺(tebufenpyrad)、唑虫酰胺(tolfenpyrad)、flufenerim;
A.9.METI II和III化合物:灭醌螨(acequinocyl)、fluacyprim、灭蚁腙(hydramethylnon);
A.10.去偶化合物:氟唑虫清(chlorfenapyr);
A.11.起氧化磷酸化抑制剂作用的化合物:三环锡(cyhexatin)、杀螨硫隆(diafenthiuron)、杀螨锡(fenbutatin oxide)、克螨特(propargite);
A.12.蜕皮抑制剂化合物:cryomazine;
A.13.混合功能氧化酶抑制剂化合物:增效醚(piperonyl butoxide);
A.14.钠通道阻断剂化合物:噁二唑虫(indoxacarb)、metaflumizone;
A.15.其他:benclothiaz、联苯肼酯(bifenazate)、杀螟丹(cartap)、氟啶虫酰胺(flonicamid)、啶虫丙醚(pyridalyl)、拒嗪酮(pymetrozine)、硫、硫环杀(thiocyclam)、氟虫酰胺(flubendiamide)、cyenopyrafen、吡氟硫磷(flupyrazofos)、丁氟螨酯(cyflumetofen)、amidoflumet、式Γ4的氨基喹唑啉化合物:
N-R’-2,2-二halo-1-R”-环丙烷甲酰胺2-(2,6-二氯-α,α,α-三氟对甲苯基)腙或N-R’-2,2-二(R”’)-丙酰胺2-(2,6-二氯-α,α,α-三氟对甲苯基)腙,其中R’为甲基或乙基,halo为氯或溴,R”为氢或甲基且R”’为甲基或乙基;式Г5的邻氨基苯甲酰胺化合物:
其中A1为CH3、Cl、Br或I,X为C-H、C-Cl、C-F或N,Y′为F、Cl或Br,Y”为H、F、Cl或CF3,B1为氢、Cl、Br、I或CN,B2为Cl、Br、CF3、OCH2CF3或OCF2H且RB为氢、CH3或CH(CH3)2,以及如JP2002284608、WO 02/89579、WO 02/90320、WO 02/90321、WO 04/06677、WO 04/20399、JP 200499597、WO 05/68423、WO 05/68432或WO05/63694所述的丙二腈化合物,特别是如下丙二腈化合物:CF3(CH2)2C(CN)2CH2(CF2)3CF2H、CF3(CH2)2C(CN)2CH2(CF2)5CF2H、CF3(CH2)2C(CN)2(CH2)2C(CF3)2F、CF3(CH2)2C(CN)2(CH2)2(CF2)3CF3、CF2H(CF2)3CH2C(CN)2CH2(CF2)3CF2H、CF3(CH2)2C(CN)2CH2(CF2)3CF3、CF3(CF2)2CH2C(CN)2CH2(CF2)3CF2H和CF3CF2CH2C(CN)2CH2(CF2)3CF2H。
A组的市售化合物可在其它出版物中,在The Pesticide Manual,第13版,British Crop Protection Council(2003)中找到。式Γ2的硫代酰胺及其合成已经描述在WO 98/28279中。Lepimectin由Agro Project,PJBPublications Ltd,2004年11月已知。Benclothiaz及其其合成已经描述在EP-A1454621中。杀扑磷(methidathion)和对氧磷(Paraoxon)及其合成已经描述在Farm Chemicals Handbook,第88卷,Meister PublishingCompany,2001中。Acetoprole及其合成已经描述在WO 98/28277中。氰氟虫胺(metaflumizone)及其合成已经描述在EP-A1462456中。Flupyrazofos已经描述在Pesticide Science 54,1988,第237-243页和US 4822779中。Pyrafluprole及其合成已经描述在JP 2002193709和WO 01/00614中。Pyriprole及其合成已经描述在WO 98/45274和US6,335,357中。Amidoflumet及其合成已经描述在US 6,221,890和JP 21010907中。Flufenerim及其合成已经描述在WO 03/007717和WO 03/007718中。丁氟螨酯(cyflumetofen)及其合成已经描述在WO04/080180中。式Г5的邻氨基苯甲酰胺(anthranilamide)及其合成已经描述在WO 01/70671;WO 02/48137;WO 03/24222、WO 03/15518、WO04/67528;WO 04/33468和WO 05/118552中。丙二腈化合物CF3(CH2)2C(CN)2CH2(CF2)3CF2H、CF3(CH2)2C(CN)2CH2(CF2)5CF2H、CF3(CH2)2C(CN)2(CH2)2C(CF3)2F、CF3(CH2)2C(CN)2(CH2)2(CF2)3CF3、CF2H(CF2)3CH2C(CN)2CH2(CF2)3CF2H、CF3(CH2)2C(CN)2CH2(CF2)3CF3、CF3(CF2)2CH2C(CN)2CH2(CF2)3CF2H和CF3CF2CH2C(CN)2CH2(CF2)3CF2H已经描述在WO 05/63694中。
具有杀真菌活性的活性物质的实例在组B.1-B.6中提到:
B.1.嗜球果伞素类(Strobilurins),如腈嘧菌酯(azoxystrobin)、醚菌胺(dimoxystrobin)、烯肟菌酯(enestroburin)、氟嘧菌酯(fluoxastrobin)、亚胺菌(kresoxim-methyl)、叉氨苯酰胺(metominostrobin)、啶氧菌酯(picoxystrobin)、唑菌胺酯(pyraclostrobin)、肟菌酯(trifloxystrobin)、肟醚菌胺(orysastrobin)、(2-氯-5-[1-(3-甲基苄氧亚氨基)乙基]苄基)氨基甲酸甲酯、(2-氯-5-[1-(6-甲基吡啶-2-基甲氧基亚氨基)乙基]苄基)氨基甲酸甲酯、2-(邻-((2,5-二甲基苯氧基亚甲基)苯基)-3-甲氧基丙烯酸甲酯;
B.2羧酰胺类如:
·羧酰苯胺类:苯霜灵(benalaxyl)、麦锈灵(benodanil)、啶酰菌胺(boscalid)、萎锈灵(carboxin)、丙氧灭绣胺(mepronil)、呋菌胺(fenfuram)、环酰菌胺(fenhexamide)、氟酰胺(flutolanil)、呋吡唑灵(furametpyr)、甲霜灵(metalaxyl)、甲呋酰胺(ofurace)、噁霜灵(oxadixyl)、氧化萎锈灵(oxycarboxin)、吡噻菌胺(penthiopyrad)、溴氟唑菌(thifluzamide)、噻酰菌胺(tiadinil)、N-(4’-溴联苯-2-基)-4-二氟甲基-2-甲基噻唑-5-甲酰胺、N-(4’-三氟甲基联苯-2-基)-4-二氟甲基-2-甲基噻唑-5-甲酰胺、N-(4’-氯-3’-氟联苯-2-基)-4-二氟甲基-2-甲基噻唑-5-甲酰胺、N-(3’,4’-二氯-4-氟联苯-2-基)-3-二氟甲基-1-甲基吡唑-4-甲酰胺、N-(2-氰基苯基)-3,4-二氯异噻唑-5-甲酰胺、2-氨基-4-甲基噻唑-5-甲酰苯胺、2-氯-N-(1,1,3-三甲基茚满-4-基)烟酰胺、N-(2’,4’-二氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2’,4’-二氯联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2’,5’-二氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2’,5’-二氯联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3’,5’-二氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3’,5’-二氯联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3’-氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3’-氯联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2’-氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2’-氯联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3’,4’,5’-三氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2’,4’,5’-三氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-[2-(1,1,2,3,3,3-六氟丙氧基)苯基]-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-[2-(1,1,2,2-四氟乙氧基)苯基]-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(4’-三氟甲硫基联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3’,4’-二氯-5-氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2-(1,3-二甲基丁基)苯基)-1,3,3-三甲基-5-氟-1H-吡唑-4-甲酰胺、N-(4’-氯-3’,5’-二氟联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(4’-氯-3’,5’-二氟联苯-2-基)-3-三氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3’,4’-二氯-5’-氟联苯-2-基)-3-三氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3’,5’-二氟-4’-甲基联苯-2-基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(3’,5’-二氟-4’-甲基联苯-2-基)-3-三氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(2-双环丙-2-基-苯基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(顺-2-双环丙-2-基-苯基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺、N-(反-2-双环丙-2-基-苯基)-3-二氟甲基-1-甲基-1H-吡唑-4-甲酰胺;
·羧酸吗啉化物:烯酰吗啉(dimethomorph)、氟吗啉(flumorph);
·苯甲酰胺类:氟联苯菌(flumetover)、fluopicolide(氟吡菌胺(picobenzamid))、苯酰菌胺(zoxamide);
·其他羧酰胺:氯环丙酰胺(carpropamid)、双氯氰菌胺(diclocymet)、双炔酰菌胺(mandipropamid)、N-(2-(4-[3-(4-氯苯基)丙-2-炔氧基]-3-甲氧基苯基)乙基)-2-甲烷磺酰基氨基-3-甲基丁酰胺、N-(2-(4-[3-(4-氯苯基)丙-2-炔氧基]-3-甲氧基苯基)乙基)-2-乙烷磺酰基氨基-3-甲基丁酰胺;
B.3.唑类:
·三唑类:双苯三唑醇(bitertanol)、糠菌唑(bromuconazole)、环唑醇(cyproconazole)、噁醚唑(difenoconazole)、烯唑醇(diniconazole)、烯菌灵(enilconazole)、氧唑菌(epoxiconazole)、腈苯唑(fenbuconazole)、氟硅唑(flusilazole)、喹唑菌酮(fluq uinconazole)、粉唑醇(flutriafol)、己唑醇(hexaconazole)、酰胺唑(imibenconazole)、环戊唑醇(ipconazole)、环戊唑菌(metconazole)、腈菌唑(myclobutanil)、戊菌唑(penconazole)、丙环唑(propiconazole)、丙硫菌唑(prothioconazole)、硅氟唑(simeconazole)、戊唑醇(tebuconazole)、氟醚唑(tetraconazole)、唑菌醇(triadimenol)、三唑酮(triadimefon)、戊叉唑菌(triticonazole)、戊环菌(azaconazole)、烯唑醇(diniconazole-M)、oxpoconazole、paclobutrazole、烯效唑(uniconazole)、1-(4-氯苯基)-2-([1,2,4]三唑-1-基)环庚醇;
·咪唑类:氰霜唑(cyazofamid)、烯菌灵(imazalil)、稻瘟酯(pefurazoate)、丙氯灵(prochloraz)、氟菌唑(triflumizole);
·苯并咪唑类:苯菌灵(benomyl)、多菌灵(carbendazim)、麦穗宁(fuberidazole)、涕必灵(thiabendazole);
·其他:噻唑菌胺(ethaboxam)、氯唑灵(etridiazole)、土菌消(hymexazole);
B.4.含氮杂环基化合物如:
·吡啶类:氟啶胺(fluazinam)、啶斑肟(pyrifenox)、3-[5-(4-氯苯基)-2,3-二甲基异噁唑烷-3-基]吡啶;
·嘧啶类:磺嘧菌灵(bupirimate)、环丙嘧啶(cyprodinil)、嘧菌腙(ferimzone)、异嘧菌醇(fenarimol)、嘧菌胺(mepanipyrim)、氟苯嘧啶醇(nuarimol)、二甲嘧菌胺(pyrimethanil);
·哌嗪类:嗪氨灵(triforine);
·吡咯类:氟噁菌(fludioxonil)、拌种咯(fenpiclonil);
·吗啉类:4-十二烷基-2,6-二甲基吗啉(aldimorph)、吗菌灵(dodemorph)、丁苯吗啉(fenpropimorph)、克啉菌(tridemorph);
·二羧酰亚胺类:异丙定(iprodione)、杀菌利(procymidone)、烯菌酮(vin clozolin);
·其他:噻二唑素(acibenzolar-S-methyl)、敌菌灵(anilazine)、克菌丹(captan)、敌菌丹(captafol)、棉隆(dazomet)、哒菌清(diclomezine)、氰菌胺(fenoxanil)、灭菌丹(folpet)、苯锈啶(fenpropidin)、噁唑酮菌(famoxadone)、咪唑菌酮(fenamidone)、异噻菌酮(octhilinone)、噻菌灵(probenazole)、丙氧喹啉(proquinazid)、咯喹酮(pyroquilon)、喹氧灵(quinoxyfen)、三环唑(tricyclazole)、5-氯-7-(4-甲基哌啶-1-基)-6-(2,4,6-三氟苯基)-[1,2,4]三唑并[1,5-a]嘧啶、2-丁氧基-6-碘-3-丙基苯并吡喃-4-酮、N,N-二甲基-3-(3-溴-6-氟-2-甲基吲哚-1-磺酰基)-[1,2,4]三唑-1-磺酰胺;
B.5.氨基甲酸盐和二硫代氨基甲酸盐如:
·二硫代氨基甲酸盐:福美铁(ferbam)、代森锰锌(maneozeb)、代森锰(maneb)、代森联(metiram)、威百亩(metam)、甲基代森锌(propineb)、福美双(thiram)、代森锌(zineb)、福美锌(ziram);
·氨基甲酸盐类:乙霉威(diethofencarb)、flubenthiavalicarb、异丙菌胺(iprovalicarb)、百维灵(propamocarb)、3-(4-氯苯基)-3-(2-异丙氧羰基氨基-3-甲基丁酰氨基)丙酸甲酯、N-(1-(1-(4-氰基苯基)乙烷磺酰基)丁-2-基)氨基甲酸4-氟苯基酯;
6.其他杀真菌剂如:
·胍类:多果定(dodine)、双胍辛醋酸盐(iminoctadine)、双胍盐(guazatine);
·抗菌素类:春雷素(kasugamycin)、多氧霉素(polyoxins)、链霉素(streptomycin)、井冈霉素(validamycin A);
·有机金属化合物类:三苯锡基盐;
·含硫的杂环基化合物:稻瘟灵(isoprothiolane)、二噻农(dithianon);
·有机磷化合物:克瘟散(edifenphos)、藻菌磷(fosetyl)、乙膦铝(fosetyl-aluminum)、异稻瘟净(iprobenfos)、定菌磷(pyrazophos)、甲基立枯磷(tolclofos-methyl)、亚磷酸及其盐;
·有机氯化合物:甲基托布津(thiophanate-methyl)、百菌清(chlorothalonil)、抑菌灵(dichlofluanid)、对甲抑菌灵(tolylfluanid)、磺菌胺(flusulfamide)、四氯苯酞(phthalide)、六氯苯(hexachlorobenzene)、戊菌隆(pencycuron)、五氯硝基苯(quintozene);
·硝基苯基衍生物:乐杀螨(binapacryl)、敌螨普(dinocap)、敌螨通(dinobuton);
·无机活性物质:波尔多液(Bordeaux混合物)、醋酸铜、氢氧化铜、王铜(copper oxychloride)、碱式硫酸铜、硫;
·其他:螺噁茂胺(spiroxamine)、环氟菌胺(cyflufenamid)、清菌脲(cymoxanil)、苯菌酮(metrafenon)。
具有除草活性的活性物质的实例在组C.1-C.15中提到:
C.1类脂生物合成抑制剂,如炔禾灵(chlorazifop)、炔草酯(clodinafop)、氯丁草(clofop)、氰氟草酯(cyhalofop)、氯甲草(diclofop)、噁唑禾草灵(fenoxaprop)、高噁唑禾草灵(fenoxaprop-p)、噻唑禾草灵(fenthiaprop)、吡氟禾草灵(fluazifop)、精吡氟禾草灵(fluazifop-P)、吡氟氯禾灵(haloxyfop)、精吡氟氯禾灵(haloxyfop-P)、恶草醚(isoxapyrifop)、噁唑酰草胺(metamifop),喔草酯(propaquizafop)、喹禾灵(quizalofop)、精喹禾灵(quizalofop-P)、三氟苯氧丙酸(trifop)、枯杀达(alloxydim)、丁氧环酮(butroxydim)、烯草酮(clethodim)、环己烯草酮(cloproxydim)、噻草酮(cycloxydim)、环苯草酮(profoxydim)、稀禾定(sethoxydim)、醌肟草(tepraloxydim)、肟草酮(tralkoxydim)、苏达灭(butylate)、草灭特(cycloate)、燕麦敌(di-allate)、哌草丹(dimepiperate)、扑草灭(EPTC)、禾草畏(esprocarb)、抑草威(ethiolate)、氮草(isopolinate)、甲硫苯威(methiobencarb)、草达灭(molinate)、坪草丹(orbencarb)、克草猛(pebulate)、苄草丹(prosulfocarb)、草克死(sulfallate)、杀草丹(thiobencarb)、丁草威(thiocarbazil)、野麦畏(tri-allate)、灭草猛(vernolate)、呋草黄(benfuresate)、乙呋草黄(ethofumesate)和地散磷(bensulide);
C.2ALS抑制剂,如磺氨黄隆(amidosulfuron)、四唑黄隆(azimsulfuron)、苄嘧黄隆(bensulfuron)、氯嘧黄隆(chlorimuron)、绿黄隆(chlorsulfuron)、醚黄隆(cinosulfuron)、环丙黄隆(cyclosulfamuron)、胺苯黄隆(ethametsulfuron)、乙氧嘧黄隆(ethoxysulfuron)、啶嘧黄隆(flazasulfuron)、氟定黄隆(flupyrsulfuron)、甲酰氨磺隆(foramsulfuron)、吡氯黄隆(halosulfuron)、啶咪黄隆(imazosulfuron)、碘黄隆(iodosulfuron)、甲基二磺隆(mesosulfuron)、甲黄隆(metsulfuron)、烟嘧黄隆(nicosulfuron)、环丙氧黄隆(oxasulfuron)、氟嘧黄隆(primisulfuron)、氟丙黄隆(prosulfuron)、吡嘧黄隆(pyrazosulfuron)、玉嘧黄隆(rimsulfuron)、嘧黄隆(sulfometuron)、乙黄黄隆(sulfosulfuron)、噻黄隆(thifensulfuron)、醚苯黄隆(triasulfuron)、苯黄隆(tribenuron)、三氟啶磺隆(trifloxysulfuron)、氟胺磺隆(triflusulfuron)、三氟甲磺隆(tritosulfuron)、咪草酯(imazamethabenz)、咪草啶酸(imazamox)、甲基咪草烟(imazapic)、灭草烟(imazapyr)、灭草喹(imazaquin)、咪草烟(imazethapyr)、唑嘧磺胺盐(cloransulam)、唑嘧磺胺(diclosulam)、双氟磺草胺(florasulam)、氟唑啶草(flumetsulam)、唑草磺胺(metosulam)、五氟磺草胺(penoxsulam)、双嘧苯甲酸(bispyribac)、肟啶草(pyriminobac)、丙苯磺隆(propoxycarbazone)、氟酮磺隆(flucarbazone)、嘧苯草肟(pyribenzoxim)、环酯草醚(pyriftalid)和嘧硫苯甲酸(pyrithiobac);
C.3光合成抑制剂,如莠去通(atraton)、莠去津(atrazine)、莠灭净(ametryn)、叠氮津(aziprotryn)、草净津(cyanazine)、硫草净津(cyanatryn)、可乐津(chlorazine)、环草津(cyprazine)、敌草净(desmetryn)、戊草津(dimethametryn)、杀草净(dipropetryn)、草止津(eglinazine)、抑草津(ipazine)、麦苏百津(mesoprazine)、醚草通(methometon)、盖草津(methoprotryne)、环氰津(procyazine)、丙草止津(proglinazine)、扑灭通(prometon)、扑草净(prometryn)、扑灭津(propazine)、另丁津(sebuthylazine)、密草通(secbumeton)、西玛津(simazine)、西玛通(simeton)、西草净(simetryn)、甲氧去草净(terbumeton)、特丁津(terbuthylazine)、去草净(terbutryn)、草达津(trietazine)、特津酮(ametridione)、特草嗪酮(amibuzin)、六嗪同(hexazinone)、嗪丁草(isomethiozin)、苯嗪草(metamitron)、赛克津(metribuzin)、除草定(bromacil)、异草定(isocil)、环草定(lenacil)、特草定(terbacil)、溴杀草敏(brompyrazon)、杀草敏(chloridazon)、敌米达松(dimidazon)、异苯敌草(desmedipham)、敌克草(phenisopham)、苯敌草(phenmedipham)、乙苯敌草(phenmedipham-ethyl)、噻草隆(benzthiazuron)、丁噻隆(buthiuron)、噻二唑隆(ethidimuron)、异恶隆(isouron)、噻唑隆(methabenzthiazuron)、monoisouron、丁唑隆(tebuthiuron)、赛唑隆(thiazafluron)、疏草隆(anisuron)、播土隆(buturon)、氯溴隆(chlorbromuron)、乙氧苯隆(chloreturon)、绿麦隆(chlorotoluron)、枯草隆(chloroxuron)、枯莠隆(difenoxuron)、丁噁隆(dimefuron)、敌草隆(diuron)、非草隆(fenuron)、伏草隆(fluometuron)、氟苯隆(fluothiuron)、异丙隆(isoproturon)、利谷隆(linuron)、灭草恒(methiuron)、色满隆(metobenzuron)、秀谷隆(metobromuron)、甲氧隆(metoxuron)、绿谷隆(monolinuron)、灭草隆(monuron)、草不隆(neburon)、对伏隆(parafluron)、稀草隆(phenobenzuron)、环草隆(siduron)、氟氧隆(tetrafluron)、赛二唑素(thidiazuron)、莎草快(cyperquat)、二乙除草双(diethamquat)、苯敌快(difenzoquat)、敌草快(diquat)、伐草快(morfamquat)、对草快(paraquat)、糠草腈(bromobonil)、溴苯腈(bromoxynil)、羟敌草腈(chloroxynil)、碘草腈(iodobonil)、碘苯腈(ioxynil)、氨唑草酮(amicarbazone)、杀草全(bromofenoxim)、三氟噁嗪(flumezin)、灭草定(methazole)、噻草平(bentazone)、敌稗(propanil)、蔬草灭(pentanochlor)、达草止(pyridate)和6-氯-3-苯基-4-哒嗪醇(pyridafol);
C.4原卟啉原-IX氧化酶抑制剂,如氟锁草醚(acifluorfen)、治草醚(bifenox)、氯硝醚(chlomethoxyfen)、草枯醚(chlornitrofen)、氯氟草醚(ethoxyfen)、消草醚(fluorodifen)、乙羧氟草醚(fluoroglycofen)、氯草醚(fluoronitrofen)、氟黄胺草醚(fomesafen)、氟呋草醚(furyloxyfen)、氟硝磺酰胺(halosafen)、乳氟禾草灵(lactofen)、除草醚(nitrofen)、硝氟草醚(nitrofluorfen)、氟硝草醚(oxyfluorfen)、异丙吡草酯(fluazolate)、氟唑草酯(pyraflufen)、吲哚酮草酯(cinidon-ethyl)、酰亚胺苯氧乙酸(flumiclorac)、氟噁嗪酮(flumioxazin)、炔草胺(flumipropyn)、达草氟(fluthiacet)、噻二唑胺(thidiazimin)、恶草灵(oxadiazon)、炔丙噁唑草(oxadiargyl)、唑啶炔草(azafenidin)、氟酮唑草(carfentrazone)、磺胺草唑(sulfentrazone)、戊噁唑草(pentoxazone)、双苯嘧草酮(benzfendizone)、氟丙嘧草酯(butafenacil)、双唑草腈(pyraclonil)、氟唑草胺(profluazol)、氟哒嗪草酯(flufenpyr)、flupropacil、吡氯草胺(nipyraclofen)和乙胺草醚(etnipromid);
C.5漂白剂除草剂,如氟哒草(metflurazon)、达草灭(norflu razon)、氟苯啶草(flufenican)、吡氟草胺(diflufenican)、氟吡酰草胺(picolinafen)、氟丁酰草胺(beflubutamid)、氟草同(fluridone)、氟咯草酮(flurochloridone)、呋草酮(flurtamone)、甲基磺草酮(mesotrione)、磺草酮(sulcotrione)、异恶氯草酮(isoxachlortole)、异噁氟草(isoxaflutole)、吡草酮(benzofenap)、吡唑特(pyrazolynate)、苄草唑(pyrazoxyfen)、苯并双环酮(benzobicyclon)、杀草强(amitrole)、异恶草酮(clomazone)、苯草醚(aclonifen)、4-(3-三氟甲基苯氧基)-2-(4-三氟甲基苯基)嘧啶以及式II的3-杂环基取代的苯甲酰基衍生物(参见WO-A-96/26202、WO-A-97/41116、WO 97/41117和WO97/41118):
其中变量R8-R13具有如下含义:
R8、R10为氢、卤素、C1-C6烷基、C1-C6卤代烷基、C1-C6烷氧基、C1-C6卤代烷氧基、C1-C6烷硫基、C1-C6烷基亚磺酰基或C1-C6烷基磺酰基;
R9为选自如下的杂环基:噻唑-2-基、噻唑-4-基、噻唑-5-基、异噁唑-3-基、异噁唑-4-基、异噁唑-5-基、4,5-二氢异噁唑-3-基、4,5-二氢异噁唑-4-基和4,5-二氢异噁唑-5-基,其中九个所述基团例如可以未被取代或被卤素、C1-C4烷基、C1-C4烷氧基、C1-C4卤代烷基、C1-C4卤代烷氧基或C1-C4烷硫基单取代或多取代,如单-、二-、三或四取代;
R11为氢、卤素或C1-C6烷基;
R12为C1-C6烷基;
R13为氢或C1-C6烷基。
C.6EPSP合成酶抑制剂,如草甘膦(glyphosate);
C.7谷氨酰胺合成酶抑制剂,如草铵膦(glufosinate)和双丙氨酰磷(bilanafos);
C.8DHP合成酶抑制剂,如黄草灵(asulam);
C.9有丝分裂抑制剂,如氟草胺(benfluralin)、地乐胺(butralin)、敌乐胺(dinitramine)、丁氟消草(ethalfluralin)、氟消草(fluchloralin)、异乐灵(isopropalin)、氟烯硝草(methalpropalin)、磺乐灵(nitralin)、黄草消(oryzalin)、胺硝草(pendimethalin)、氨基丙氟灵(prodiamine)、卡乐施(profluralin)、氟乐灵(trifluralin)、甲基胺草磷(amiprofos-methyl)、草胺磷(butamifos)、氟硫草定(dithiopyr)、噻氟啶草(thiazopyr)、拿草特(propyzamide)、丙戊草胺(tebutam)、敌草索(chlorthal)、长杀草(carbetamide)、氯草灵(chlorbufam)、氯苯胺灵(chlorpropham)和苯胺灵(propham);
C.10VLCFA抑制剂,如乙草胺(acetochlor)、甲草胺(alachlor)、丁草胺(butachlor)、丁烯草胺(butenachlor)、敌草乐(delachlor)、安塔(diethatyl)、克草胺(dimethachlor)、噻吩草胺(dimethenamid)、精噻吩草胺(dimethenamid-P)、吡草胺(metazachlor)、异丙甲草胺(metolachlor)、S-异丙甲草胺(S-metolachlor)、丙草胺(pretilachlor)、扑草胺(propachlor)、异丙草胺(propisochlor)、广草胺(prynachlor)、猛杀草(terbuchlor)、噻醚草胺(thenylchlor)、二甲苯草胺(xylachlor)、草毒死(allidochlor)、草立死(CDEA)、磺唑草(epronaz)、草乃敌(diphenamid)、草萘胺(napropamide)、萘丙胺(naproanilide)、烯草胺(pethoxamid)、氟噻草胺(flufenacet)、苯噻草胺(mefenacet)、四唑酰草胺(fentrazamide)、莎稗磷(anilofos)、哌草磷(piperophos)、胺草唑(cafenstrole)、茚草酮(indanofan)和灭草环(tridiphane);
C.11纤维素生物合成抑制剂,如敌草腈(dichlobenil)、草克乐(chlorthiamid)、异恶草胺(isoxaben)和胺草唑(flupoxam);
C.12去偶除草剂,如消草酯(dinofenate)、硝丙酚(dinoprop)、戊硝酚(dinosam)、地乐酚(dinoseb)、地乐消酚(dinoterb)、二硝甲酚(DNOC)、硝草酚(etinofen)和丁硝酚(medinoterb);
C.13植物生长素除草剂,如稗草胺(clomeprop)、2,4-滴(2,4-D)、2,4,5-涕(2,4,5-T)、2甲4氯(MCPA)、酚硫杀(MCPA-thioethyl)、2,4-滴丙酸(dichlorprop)、高2,4-滴丙酸(dichlorprop-P)、2甲4氯丙酸(mecoprop)、高2甲4氯丙酸盐(mecoprop-P)、2,4-滴丁酸(2,4-DB)、2甲4氯丁酸(MCPB)、草灭平(chloramben)、麦草畏(dicamba)、草芽平(2,3,6-TBA)、杀草畏(tricamba)、二氯喹啉酸(quinclorac)、喹草酸(quinmerac)、二氯皮考啉酸(clopyralid)、氟草烟(fluroxypyr)、毒莠定(picloram)、定草酯(triclopyr)和草除灵(benazolin);
C.14植物生长素输送抑制剂,如抑草生(naptalam)、二氟吡隆(diflufenzopyr);
C.15:新燕灵(benzoylprop)、氟燕灵(flamprop)、强氟燕灵(flamprop-M)、溴丁酰草胺(bromobutide)、氯甲丹(chlorflurenol)、环庚草醚(cinmethylin)、苯丙隆(methyldymuron)、乙苯酰草(etobenzanid)、膦铵素(fosamine)、威百亩(metam)、稗草畏(pyributicarb)、氯噁嗪草(oxaziclomefone)、棉隆(dazomet)、苯氧丙胺津(triaziflam)和溴甲烷(methylbromide)。
合适的安全剂可列举如下:
解草酮(benoxacor)、喹氧乙酸(cloquintocet)、抑害腈(cyometrinil)、抑害胺(dichlormid)、dicyclonon、dietholate、解草唑(fenchlorazole)、解草啶(fenclorim)、解草胺(flurazole)、肟草安(fluxofenim)、解草呋(furilazole)、双苯恶唑酸(isoxadifen)、吡咯二酸(mefenpyr)、mephenate、萘二甲酸酐(naphthalic anhydride)、2,2,5-三甲基-3-(二氯乙酰基)-1,3-噁唑烷(R-29148)、4-(二氯乙酰基)-1-氧杂-4-氮杂螺[4.5]癸烷(AD-67;MON 4660)和解草腈(oxabetrinil)。
生长调节剂的实例如下:1-萘乙酰胺、1-萘乙酸、2-萘氧基乙酸、坐果胺(3-CPA)、促生灵(4-CPA)、嘧啶醇(ancymidol)、蒽醌、苄胺基嘌呤(BAP)、脱叶亚磷(butifos);脱叶磷(tribufos)、地乐胺(butralin)、氯甲丹(chlorflurenol)、矮壮素阳离子(chlormequat)、苯哒酮酸(clofencet)、环丙酸酰胺(cyclanilide)、丁酰肼(daminozide)、麦草畏(dicamba)、敌草克钠盐(dikegulac-sodium)、噻节因(dimethipin)、敌螨(chlorfenethol)、硅长素(etacelasil)、乙烯利(ethephon)、ethychlozate、2,4,5-涕丙酸(fenoprop)、2,4,5-涕丙酸(2,4,5-TP)、氟磺胺素(fluoridamid)、调嘧醇(flurprimidol)、粉唑醇(flutriafol)、赤霉酸、赤霉素、双胍盐(guazatine)、吲哚丁酸、吲哚乙酸、karetazan、动力精(kinetin)、lactidichlor-ethyl、抑芽丹(maleichydrazide)、氟草磺(mefluidide)、甲哌鎓(mepiquat chloride)、抑草生(naptalam)、多效唑(paclobutrazol)、调环酸钙(prohexadione-calcium)、喹草酸(quinmerac)、sintofen、调环烯(tetcyclacis)、赛二唑素(thidiazuron)、三碘苯甲酸、抑芽唑(triapenthenol)、triazethan、脱叶磷(tribufos)、抗倒酯(trinexapac-ethyl)、烯效唑(uniconazole)。
肥料的实例包括硝酸钾,硫酸钾,尿素,硝酸铵,磷酸一钾,磷酸二铵,过磷酸盐,磷酸一铵,磷酸二铵,聚磷酸铵,二氧化钾,氯化钾;硝酸钙,硫酸钙,磷酸钙,硫酸镁,硝酸镁,木素磺酸镁,硫酸铵,元素硫,硼砂,硼酸钠,硫酸铜,EDTA-Cu(NH4)2,EDTA-CuNa2,氧化铁,二氧化铁,磷酸铁,硫酸铁,木素磺酸铁,EDTA-FeK,EDTA-FeNa3H2O,EDTA-FeNH4NH4OH,DTPA-FeNa2,DTPA-Fe(NH4)2,DTPA-FeNa2,DTPA-FeHNa,HEDTA-Fe,HEDTA-Fe,HEDTA-Fe,EDDHA-FeNa,EDDHA-FeNa,硫酸锰,氯化锰,氧化锰,木素磺酸锰,或锰螯合物(manganese chelate),如EDTA-MnK2、EDTA-MnNa2,钼酸钠,钼酸钾,氧化锌,硫酸锌,硫酸氧锌(zinc oxysulfate),木素磺酸锌,锌螯合物(zincchelate)如EDTA-Zn(NH4)2、EDTA-ZnNa2,二氧化硒,磷酸硒或氯化硒。
关于种子处理,植物保护剂优选选自具有杀真菌、杀昆虫、杀螨和/或杀线虫活性的有机活性物质。它们尤其为一种或多种如下物质:
具有杀虫或杀螨或杀线虫活性的物质,其尤其选自:吡虫清(acetamiprid)、甲体氯氰菊酯(alpha-cypermethrin)、乙体氯氰菊酯(beta-cypermethrin)、氟氯菊酯(bifenthrin)、虫螨威(carbofuran)、丁硫克百威(carbosulfan)、噻虫胺(clothianidin)、乙氰菊酯(cycloprothrin)、氟氯氰菊酯(cyfluthrin)、氯氰菊酯(cypermethrin)、溴氰菊酯(deltamethrin)、氟脲杀(diflubenzuron)、呋虫胺(dinotefuran)、醚菊酯(etofenprox)、杀螨锡(fenbutatin oxide)、甲氰菊酯(fenpropathrin)、锐劲特(fipronil)、氟氰戊菊酯(flucythrinate)、吡虫啉(imidacloprid)、λ-氯氟氰菊酯(Lambda-Cyhalothrin)、硝胺烯啶(nitenpyram)、信息素、艾克敌105(spinosad)、伏虫隆(teflubenzuron)、七氟菊酯(tefluthrin)、特丁磷(terbufos)、噻虫啉(thiacloprid)、噻虫嗪(thiamethoxam)、硫双灭多威(thiodicarb)、四溴菊酯(tralomethrin)、唑蚜威(triazamate)、己体氯氰菊酯(zeta-cypermethrin)、spirotetramate、吡氟硫磷(flupyrazofos)、NC512、唑虫酰胺(tolfenpyrad)、氟虫酰胺(flubendiamide)、双三氟虫脲(bistrifluron)、benclothiaz、DPX-E2Y45、HGW86、pyrafluprol、pyriprol、F-7663、F-2704、amidoflumet、flufenerim和丁氟螨酯(cyflumetofen)。
具有杀真菌活性的物质,例如甲霜灵(metalaxyl)、噁霜灵(oxadixyl)、双胍盐(guazatine)、二甲嘧菌胺(pyrimethanil)、链霉素(streptomycin),来自B.3的杀真菌剂,尤其是三唑类如噁醚唑(difenoconazole)、氧唑菌(epoxiconazole)、喹唑菌酮(fluquinconazole)、粉唑醇(flutriafol)、土菌消(hymexazol)、烯菌灵(imazalil)、环戊唑菌(metconazole)、丙氯灵(prochloraz)、丙硫菌唑(prothioconazole)、戊唑醇(tebuconazole)、涕必灵(thiabendazole)、唑菌醇(triadimenol)或戊叉唑菌(triticonazole),还有异丙定(iprodion)、代森锰(maneb)、代森锰锌(mancozeb)、代森联(metiram)、福美双(thiram)、苯菌灵(benomyl)、啶酰菌胺(boscalid)、多菌灵(carbendazim)、萎锈灵(carboxin)、棉隆(dazomet)、硅噻菌胺(silthiofam)、铜类杀真菌剂、氟噁菌(fludioxonil)、硫、棉隆(dazomet)、B1组的杀真菌剂,尤其是腈嘧菌酯(azoxystrobin)、亚胺菌(kresoxim-methyl)、肟醚菌胺(orysastrobin)、唑菌胺酯(pyraclostrobin)或肟菌酯(trifloxystrobin),以及克菌丹(captan)或烯酰吗啉(dimethomorph)。
上述植物保护剂可单独或相互组合使用。
含活性物质颗粒中植物保护剂的总量基于活性物质颗粒组分的总量通常为1-30重量%,经常5-30重量%,尤其是8-25重量%。聚合物P与植物保护剂的比例优选为至少1∶1,尤其是2∶1-10∶1。
本发明的优选实施方案为如下活性物质组合物,其中所述至少一种植物保护剂包含至少一种杀真菌剂,尤其是至少一种优选的杀真菌剂,尤其是至少一种称作组B.3的唑类杀真菌剂,且尤其在这些中选择。在该优选实施方案中,聚合物P优选选自聚丙交酯、聚己内酯、聚丙交酯与聚C2-C4亚烷基二醇,特别是与聚乙二醇的嵌段共聚物,以及聚己内酯与聚C2-C4亚烷基二醇,特别是与聚乙二醇的嵌段共聚物。该实施方案的特别优选的聚合物P为聚己内酯,尤其是数均分子量为50000-100000g/mol的那些,特别优选数均分子量为80000-100000g/mol的那些。该实施方案的特别优选的聚合物P也为聚己内酯与聚C2-C4亚烷基二醇,特别是与聚乙二醇的嵌段共聚物,尤其是数均分子量为50000-100000g/mol的那些,特别优选数均分子量为80000-100000g/mol的那些。
存在于活性物质组合物中的酶的类型以本身已知的方式取决于可酶促降解聚合物P的类型。根据本发明,所述至少一种酶为水解酶,即通过加入水能够水解裂解化学键的酶。
合适的酶分类的实例详述如下:
能够使酯键水解的酶(酯酶:酶分类EC 3.1),如EC分类的酶
EC 3.1.1(羧酸酯水解酶),
EC 3.1.2(硫代酸酯水解酶),
EC 3.1.3(磷酸单酯水解酶),
EC 3.1.4(磷酸二酯水解酶),
EC 3.1.5(三磷酸单酯水解酶),
EC 3.1.6(硫酸酯水解酶),
EC 3.1.7(二磷酸单酯水解酶),
EC 3.1.8(磷酸三酯水解酶);
糖基酶(glycosylases)(EC 3.2),例如来自EC分类的糖基酶,
EC 3.2.1(糖苷酶,即使O-和S-糖基化合物水解的酶),
EC 3.2.2(使N-糖基化合物水解的酶),
EC 3.2.3(使S-糖基化合物水解的酶);
使醚键水解的酶(EC 3.3),例如来自EC分类的酶
EC 3.3.1(硫醚和三烷基锍水解酶)
EC 3.3.2(醚水解酶)
使肽键水解的酶,即肽酶(EC 3.4),例如来自EC分类的肽酶
EC 3.4.11(氨基肽酶)
EC 3.4.13(二肽酶)
EC 3.4.14(二肽基肽酶和三肽基肽酶)
EC 3.4.15(肽基二肽酶)
EC 3.4.16(丝氨酸类羧基肽酶)
EC 3.4.17(金属羧基肽酶(metallocarboxypeptidases))
EC 3.4.18(半胱氨酸类羧基肽酶)
EC 3.4.19(ω-肽酶)
EC 3.4.21(丝氨酸肽链内切酶)
EC 3.4.22(半胱氨酸肽链内切酶)
EC 3.4.23(天冬氨酸肽链内切酶)
EC 3.4.24(金属肽链内切酶)
EC 3.4.25(苏氨酸肽链内切酶)
EC 3.4.99(具有未知催化机理的肽链内切酶)
使非酰胺键的碳-氮键水解的酶(EC 3.5),例如来自EC分类的酶
EC 3.5.1(使线性酰胺催化水解的酶)
EC 3.5.2(使环酰胺催化水解的酶)
EC 3.5.3(使线性脒催化水解的酶)
EC 3.5.4(使环脒催化水解的酶)
EC 3.5.99(使其它化合物催化水解的酶)
使酸酐水解的酶(EC3.6),例如EC分类的酶
EC 3.6.1(使含磷的酸酐催化水解的酶)
EC 3.6.2(使含磺酰基酸酐催化水解的酶)
EC 3.6.3(对酸酐具有催化活性的酶)
EC 3.6.4(对酸酐具有催化活性的酶)
EC 3.6.5(对GPT具有催化活性的酶)
使碳-碳键水解的酶(EC 3.7),例如
EC 3.7.1(使含酮底物催化水解的酶)
使卤素-碳键水解的酶(EC 3.8),例如来自EC分类的酶
EC 3.8.1(使C-卤素化合物水解的酶)
使磷-氮键水解的酶(EC3.9)
使硫-氮键水解的酶(EC3.10)
使碳-磷键水解的酶(EC3.11)
使硫-硫键水解的酶(EC3.12),和
使碳-硫键水解的酶(EC3.13)。
在上述酶中,优选来自酰胺酶(EC 3.5)、蛋白酶(EC 3.4)和酯酶(EC 3.1)的那些。
如果聚合物P为在聚合物骨架中具有多个酯基的聚合物,则酶通常为酯酶(酯分类EC 3.1.X.X),尤其是羧酸酯水解酶(酯分类EC 3.1.1.X),特别是:
-来自脂肪酶的酶(EC 3.1.1.3,三乙酰基甘油脂肪酶),例如:来自米曲霉(Aspergillus oryzae)的脂肪酶,其例如可以商品名Novozymes CaLB L由Novozyme购得;来自伯克霍尔德氏菌(Burkholderia plantarii)(=Burkholderia glumae)的脂肪酶,其例如描述在J.prakt.Chem.,1997,339,第381-384页或Swiss-Prot.No.Q05489(UniProtKB/Swiss-Prot entry)中;来自南极假丝酵母(Candida Antarctica)的脂肪酶B,其例如描述在Structure 1994,2,第293-298页或Biochemistry 24,1995,第16838-16851页中,或
-来自角质酶(cutinase)的酶,例如来自腐皮镰孢(Fusarium solani)的角质酶,例如来自Fusarium solani subsp.pisi(血红丛赤壳(Nectriahaematococca))的角质酶1,其例如描述在Nature,1992,356,第615-618页中。
在本发明的特别优选的实施方案中,酶为来自南极假丝酵母的脂肪酶,例如描述在Structure 1994,2,第293-298页或Biochemistry 24,1995,第16838-16851页中的脂肪酶。
在本发明的另一优选实施方案中,酶为来自伯克霍尔德氏菌(=Burkholderia glumae)的脂肪酶,例如描述在J.prakt.Chem.,1997,339,第381-384页或Swiss-Prot.No.Q05489(UniProtKB/Swiss-Prot entry)中的脂肪酶。
其它适合的酶为合成或天然源的相当的酶,例如修饰的脂肪酶。修饰的酶的实例为在低温下,例如在10-25℃的温度下活性增加的那些(嗜寒的酶)。所用酶也可为重组酶,即借助遗传修饰的生物体制备的酶。这类酶也包含有效(authentic)酶的同系物,例如对化学或热变性的稳定性增加,在低温下活性增加等的变型。根据本发明适合的酶还包括经受翻译后(post-translational)修饰的那些酶。
在本发明的特别优选实施方案中,酶为脂肪酶(EC 3.1.1.3、三乙酰基甘油脂肪酶)。在该优选实施方案中,聚合物P优选选自聚丙交酯,聚己内酯,聚丙交酯与聚C2-C4亚烷基二醇,特别是与聚乙二醇的嵌段共聚物,以及聚己内酯与聚C2-C4亚烷基二醇,特别是与聚乙二醇的嵌段共聚物。该实施方案的特别优选的聚合物P为聚己内酯,尤其是数均分子量为50000-100000g/mol的那些,特别优选数均分子量为80000-100000g/mol的那些。该实施方案的特别优选的聚合物P也为聚己内酯与聚C2-C4亚烷基二醇,特别是与聚乙二醇的嵌段共聚物,尤其是数均分子量为50000-100000g/mol的那些,特别优选数均分子量为80000-100000g/mol的那些。
所选酶优选为在低于10℃的温度下基本无活性的酶。所选酶优选为在15-20℃的温度下具有足以使聚合物降解的水解酶活性的酶。选择合适的酶可由熟练技术人员基于其对确定水解酶活性的温度和底物特异性的专业知识和试验而完成。
在羧基酯酶的情况下,酯酶活性的温度特异性例如可通过使用实施例中所述分析而确定,其中乙酸对硝基苯基酯在试验温度下使用试验酶而酶促水解,且对硝基苯酚的量随后通过HPLC测定。当酶在所需温度下具有100U/mg(基于乙酸对硝基苯基酯的水解)的活性时,通常提供了足够的活性。
水解酶对聚合物P的活性例如可经由分析评估,在所述分析中测定包含酶的聚合物P的缓冲悬浮液的pH的降低。这种分析的实例在实施例中详述。
自然的是,在本发明活性物质颗粒中水解酶的量取决于水解酶对可酶促降解的聚合物的活性。其量基于活性物质颗粒的组分的总量通常为0.1-10重量%,尤其是0.5-8重量%,特别是1-5重量%。
除了上述组分之外,本发明活性物质组合物的活性物质颗粒也可包含其它组分,其量基于活性物质颗粒的总量为至多70重量%,经常至多60重量%,尤其是至多50重量%或至多40重量%,特别是至多35重量%。它们尤其包括常用于粉末制剂的组分,以及水溶性聚合物。水溶性聚合物的量基于活性物质颗粒的总量通常不超过70重量%,经常60重量%,尤其是50重量%或40重量%,特别是35重量%,非常特别是30重量%,且需要的话基于活性物质颗粒的总量通常为至少0.5重量%或至少1重量%,经常至少2重量%,尤其是至少5重量%,优选至少10重量%或至少15重量%。需要的话水溶性聚合物的量基于活性物质颗粒的总量通常为1-70重量%,经常2-60重量%,尤其是5-50重量%或10-40重量%或0.5-40重量%,优选1-35重量%,特别是5-30重量%。基于活性物质颗粒的总量使用较大量,例如5-70重量%,尤其是10-65重量%或20-60重量%的水溶性聚合物,也是有利的。水溶性聚合物为本发明活性物质颗粒带来在水中的良好的可再悬浮性,其在种子处理中尤其有帮助。活性物质的过早释放不发生,或仅在有限程度上发生。
水溶性聚合物的实例为:聚乙烯基吡咯烷酮、乙烯基吡咯烷酮的共聚物,尤其是乙烯基吡咯烷酮含量为至少50重量%,尤其是至少70重量%的那些,例如乙烯基吡咯烷酮/(甲基)丙烯酸C1-C4烷基酯共聚物和乙烯基吡咯烷酮/乙酸乙烯酯共聚物;聚乙烯基甲酰胺,部分水解的聚乙烯基甲酰胺,尤其是水解程度为10-99%的那些;丙烯酸的均聚物和共聚物,尤其是丙烯酸含量为至少20重量%的那些;甲基丙烯酸的均聚物和共聚物,尤其是甲基丙烯酸含量为至少20重量%的那些;丙烯酰胺的均聚物和共聚物,尤其是丙烯酰胺含量为至少40重量%的那些;聚乙烯亚胺;聚乙烯胺;聚己内酰胺;聚乙烯醇;水解程度>50%的部分水解的聚乙酸乙烯酯;纤维素,纤维素衍生物如羟基烷基纤维素,烷基羟基烷基纤维素,羧基烷基纤维素,烷基羟基烷基纤维素乙酸酯琥珀酸酯,烷基羟基烷基纤维素乙酸酯邻苯二甲酸酯,烷基羟基烷基纤维素邻苯二甲酸酯,纤维素乙酸酯邻苯二甲酸酯;改性淀粉和淀粉衍生物,如羟基烷基淀粉,羧基烷基淀粉,焙烤(roasted)淀粉,氧化淀粉,辛烯基琥珀酸酯淀粉等;葡聚糖和聚C2-C3氧化烯,如聚氧化乙烯,聚氧化丙烯和聚氧化乙烯/聚氧化丙烯嵌段共聚物。
根据优选实施方案,水溶性聚合物选自聚乙烯基吡咯烷酮和乙烯基吡咯烷酮的共聚物,尤其是乙烯基吡咯烷酮含量为至少50重量%,尤其是至少70重量%的那些。在该优选实施方案中,聚合物P优选选自聚丙交酯,聚己内酯,聚丙交酯与聚C2-C4亚烷基二醇,特别是与聚乙二醇的嵌段共聚物,以及聚己内酯与聚C2-C4亚烷基二醇,特别是与聚乙二醇的嵌段共聚物。该实施方案的特别优选的聚合物P为聚己内酯,尤其是数均分子量为50000-100000g/mol的那些,特别优选数均分子量为80000-100000g/mol的那些。该实施方案的特别优选的聚合物P也为聚己内酯与聚C2-C4亚烷基二醇,特别是与聚乙二醇的嵌段共聚物,尤其是数均分子量为50000-100000g/mol的那些,特别优选数均分子量为80000-100000g/mol的那些。
本发明的特定实施方案涉及其中活性物质颗粒包含如下组分的活性物质组合物:
a)至少一种选自杀真菌剂的植物保护剂,尤其是至少一种选自唑类杀真菌剂(B.3)的植物保护剂,其量基于活性物质颗粒或活性物质组合物的组分的总量通常为1-30重量%,经常5-30重量%,尤其是8-25重量%;
b)至少一种聚合物P,其选自聚丙交酯,聚己内酯,聚丙交酯与聚C2-C4亚烷基二醇,特别是与聚乙二醇的嵌段共聚物,以及聚己内酯与聚C2-C4亚烷基二醇,特别是与聚乙二醇的嵌段共聚物,尤其是至少一种选自聚己内酯的聚合物P,尤其是数均分子量为50000-100000g/mol的那些,特别优选数均分子量为80000-100000g/mol的那些,以及聚己内酯与聚C2-C4亚烷基二醇,特别是与聚乙二醇的嵌段共聚物,尤其是数均分子量为50000-100000g/mol的那些,特别优选数均分子量为80000-100000g/mol的那些,其量在每种情况下基于含活性物质颗粒的组分的总量通常为20-99重量%,经常30-95重量%,优选40-95%,尤其是45-94重量%,特别是50-90重量%,非常特别是50-89重量%或50-80重量%;
c)至少一种羧酸酯水解酶(EC 3.1.1),尤其是至少一种脂肪酶(EC 3.1.1.3)或至少一种角质酶(EC 3.1.1.74),特别优选至少一种作为优选提及的脂肪酶和/或角质酶,其量基于活性物质颗粒的组分的总量通常为0.1-10重量%,尤其是0.5-8重量%,特别是1-5重量%;
d)至少一种水溶性聚合物,其优选选自聚乙烯基吡咯烷酮和乙烯基吡咯烷酮的共聚物,尤其是乙烯基吡咯烷酮含量为至少50重量%,尤其是至少70重量%的那些,其量基于活性物质颗粒的组分的总量通常为0.5-70重量%,经常1-60重量%,尤其是2-50重量%或5-40重量%,特别是10-35重量%或15-30重量%;
其中组分a)、b)和c)的总量基于活性物质颗粒的组分的总量通常占30-99.5重量%,经常40-99重量%,尤其是50-98重量%或60-95重量%,特别是65-90重量%或70-85重量%。
此外,本发明组合物可进一步包含其它组分,该其它组分适合于制备植物保护剂的粉末组合物。实例为稳定剂、盐、缓冲剂、防结块剂等。通常而言,其在活性物质组合物中的含量不超过20重量%,尤其是10重量%,且需要的话在实现所需效果所需范围内,例如基于活性物质颗粒的组分的总量为0.001-20重量%,或0.01-10重量%。
根据本发明,活性物质组合物为其中至少90重量%颗粒的直径不超过500μm,尤其是不超过400μm,优选不超过300μm,特别是不超过200μm的粉末。通常而言,至少90重量%颗粒的直径为0.1-500μm,尤其是0.2-400μm,优选0.3-300μm,特别是0.5-200μm。测定以重量%表征的粒径和粒径分布可以本身已知的方式,例如通过在可通过用水稀释粉末而获得的1重量%本发明粉末的水分散体中光散射而进行。活性物质颗粒的平均粒径(Z均,其可通过在1重量%本发明粉末的水分散体中光散射而测定)可在宽范围内变化。通常而言,所述粒径为至少0.2μm,优选至少0.3μm,特别优选至少0.5μm。平均粒径优选为0.2-450μm,优选0.3-300μm,尤其是0.5-200μm。
存在于本发明活性物质组合物中的颗粒可具有对粉末而言普遍的形态,包括核-壳形态或微胶囊形态。然而,与微胶囊相反,它们通常具有致密结构,其中聚合物基本均匀分布在整个颗粒横截面中,其中活性物质和/或酶可在颗粒内显示浓度梯度或可均匀分布。
制备本发明活性物质组合物可通过用于制备粉状物质的常规方法完成,所述粉末物质的粉末颗粒在所述范围内且包含多种组分。通常而言,将含活性物质颗粒的组分相互混合,然后通过常规方法处理,以产生细碎粉末。这种方法也是本发明的主题。
根据本发明适合的方法的实例为共沉淀法和干燥法,如喷雾干燥、流化床干燥、流化床涂覆、微粉化、Pickering分散体的制备与随后喷雾干燥等。
共沉淀例如描述在WO99/00013中,因此将其公开内容作为参考。
根据本发明的优选实施方案,制备本发明活性物质组合物通过喷雾干燥法完成。
为此,在第一步中,将含活性物质颗粒的组分在合适的溶剂或稀释剂中相互混合,或溶解。随后使所得悬浮液或溶液经受喷雾干燥方法。此处,溶剂或稀释剂借助温暖的气流而除去,其中存在于溶液或悬浮液中的活性物质颗粒的组分形成可以本身已知的方式获得的细碎粉末。作为选择,活性物质颗粒的组分可分开溶解或分散,且所得溶液或分散体可经受伴随的喷雾干燥。
在本发明活性物质组合物通过喷雾干燥方法的制备中,在第一步中,使含活性物质颗粒的组分溶解或悬浮在合适的溶剂或稀释剂中。优选溶剂为其中溶解了含活性物质颗粒的所有组分且不破坏所用水解酶的那些。
合适溶剂的实例为:
-优选具有4-10个C原子的脂族和脂环族醚,如四氢呋喃、二噁烷、乙醚、二异丙基醚、甲基叔丁基醚;
-卤代烃,如二氯甲烷、三氯甲烷、二氯乙烷;
-环状或开链碳酸酯,如碳酸亚乙酯、碳酸亚丙酯、碳酸二乙酯;
-以及上述溶剂的混合物和上述溶剂与水的混合物。
水也适合作为仅有的溶剂或稀释剂。
在第二步中,随后在合适的喷雾装置中借助温暖的气流除去溶剂。为此,在合适的装置中将溶液或分散体喷雾入温暖的气流中。以溶液或分散体喷雾可与温暖的气流并流或逆流,优选并流进行,即以与温暖的气流相同的方向进行。
适用于喷雾的装置为单-或多物质喷嘴和雾化器盘。
下文中也称作干燥气体的温暖气流的温度在进入干燥装置时通常为50-200℃,尤其是70-180℃,特别是100-160℃。当干燥气体离开干燥装置时,其温度通常为40-120℃,尤其是60-100℃。除了空气外,合适的干燥气体尤其是惰性气体如氮气、氩气或氦气,其中优选氮气。在易于挥发的溶剂的情况下,也可使用较低温度,如室温。
通常而言,喷雾干燥在适用于该目的的喷雾干燥塔中进行。此处,将待干燥溶液或分散体和干燥气体在顶部引入塔中。在塔的底部,将干燥的活性物质颗粒与气流一起排出,且用安置在下游的装置如旋风分离器(cyclone)与气流分离。除了常规的喷雾干燥之外,也可使用内或外流化床进行附聚喷雾操作(例如来自Niro的已知为FSD的技术),其中所形成的颗粒聚集产生较大物体。然而,所形成颗粒的初级粒度优选在上述范围内且尤其是不超过300μm,特别是200μm。
合适的话,尤其是当活性物质颗粒具有一定粘性时,向其提供常规的喷雾干燥辅助剂。它们是与溶液或分散体一起引入喷雾干燥装置且确保不发生聚集或结块的细碎固体。合适的细碎固体尤其为硅石,包括疏水硅石,碱金属和碱土金属硅酸盐,碱土金属铝硅酸盐,高度交联的聚乙烯基吡咯烷酮,纤维素,淀粉,高度交联的羧甲基淀粉钠或交联的羧甲基纤维素钠。这些物质的粒度通常低于100μm(D90值)。
可根据本发明获得的活性物质组合物本身可用于植物保护。通常而言,由于它们可分散在水中,也可将其掺入液体使用制剂如稀释的喷雾混合物中。
取决于存在于活性物质颗粒中的活性物质,本发明活性物质组合物可用于对抗有害植物、植物病原性真菌、对植物有害的昆虫、螨虫和线虫,以及用于控制有用植物的生长。
本发明活性物质组合物特别适合于处理种子和土壤。
在处理土壤的情况下,将合适的话呈活性物质颗粒的稀释的含水悬浮液形式的本发明组合物,引入土壤中。通常而言,引入土壤中在播种有用植物之前或之后,优选在有用植物出苗之前完成。
本发明活性物质组合物也尤其适合于处理种子。为此,将常规的,即未处理的种子或已预处理的种子用本发明活性物质组合物或活性物质组合物的含水制剂处理,所述制剂除了水和含活性物质颗粒之外,还可额外包含种子处理产品的常规成分如粘合剂,着色剂,表面活性物质如分散剂,此外还有有机和无机增稠剂、杀菌剂、防冻剂、消泡剂等。
着色剂的实例不仅有微溶于水的颜料,而且有可溶于水的染料。可以提到的实例是以若丹明B,C.I.颜料红112和C.I.溶剂红1已知的染料,以及颜料蓝15:4、颜料蓝15:3、颜料蓝15:2、颜料蓝15:1、颜料蓝80、颜料黄1、颜料黄13、颜料红112、颜料红48:2、颜料红48:1、颜料红57:1、颜料红53:1、颜料橙43、颜料橙34、颜料橙5、颜料绿36、颜料绿7、颜料白6、颜料棕25、碱性紫10、碱性紫49、酸性红51、酸性红52、酸性红14、酸性蓝9、酸性黄23、碱性红10、碱性红108。
粘合剂的实例为聚乙烯吡咯烷酮、聚乙酸乙烯酯、聚乙烯醇、部分水解的聚乙酸乙烯酯和纤基乙酸钠。
合适的表面活性剂(辅助剂、润湿剂、粘合剂、分散剂和乳化剂)为芳族磺酸,如木素磺酸(如Borrespers类型、Borregaard)、苯酚磺酸、萘磺酸(Morwet类型,Akzo Nobel)、二丁基萘磺酸(Nekal类型,BASF AG)以及脂肪酸的碱金属盐、碱土金属盐和铵盐,烷基磺酸盐和烷基芳基磺酸盐,烷基硫酸盐,月桂基醚硫酸盐和脂肪醇硫酸盐,以及硫酸化十六醇、十七醇和十八醇和脂肪醇乙二醇醚的盐,磺化萘及其衍生物与甲醛的缩合物,萘或萘磺酸与苯酚和甲醛的缩合物,聚氧乙烯辛基酚醚,乙氧基化异辛基酚、辛基酚或壬基酚,烷基苯基聚乙二醇醚,三丁基苯基聚乙二醇醚,烷基芳基聚醚醇,异十三烷醇,脂肪醇/氧化乙烯缩合物,乙氧基化蓖麻油,聚氧乙烯烷基醚或聚氧丙烯烷基醚,月桂醇聚乙二醇醚乙酸酯,山梨醇酯,木素亚硫酸盐废液,以及蛋白质,变性蛋白质,多糖(例如甲基纤维素),疏水淀粉,聚乙烯醇(Mowiol类型,Clariant),聚羧酸酯(BASF AG,Sokalan类型),聚烷氧基化物,聚乙烯胺(BASF AG,Lupamin类型),聚乙烯亚胺(BASF AG,Lupasol类型)、聚乙烯基吡咯烷酮及其共聚物。
增稠剂(即赋予配制剂以改性的流动性能的化合物,即在静态下的高粘度和在运动状态下的低粘度)的实例为多糖如黄原胶(购自Kelco的)、23(Rhone Poulenc)或(购自R.T.Vanderbilt),以及无机和有机层状矿物,如(购自Engelhardt)。
可以加入杀菌剂以用于稳定目的。杀菌剂的实例为基于二氯酚(diclorophen)和苄醇半缩甲醛(购自ICI的或购自Thor Chemie的RS和购自Rohm&Haas的MK),以及异噻唑啉酮衍生物如烷基异噻唑啉酮和苯并异噻唑啉酮(购自Thor Chemie的ActicideMBS)的杀菌剂。
防冻剂:例如为C1-C4链烷醇,如乙醇、异丙醇、正丁醇、异丁醇,以及C2-C6多元醇,如甘油、乙二醇、己二醇和/或丙二醇。
种子可通过用于处理种子的常规技术,如通过种子包衣、种子撒粉、种子浸泡和拌种处理。
根据种子处理的第一个实施方案,将种子,即能够繁殖和意欲播种的植物部分用本发明活性物质组合物或本发明活性物质组合物的含水制剂处理。就此而言,术语种子包括仁、种子、果实、块茎、插条或类似产品,尤其是仁和种子。
植物部分的处理例如可通过将植物部分与本发明活性物质组合物的含水悬浮液混合或通过用本发明种子组合物对种子撒粉而完成。这些措施可以在用于种子处理的特定设备,例如以种子条播机(drill seeder)进行。然而,处理也可以简单的方式,通过将本发明活性物质组合物的含水悬浮液与种子在容器中,例如在桶或盘中混合,随后使种子干燥而进行。
作为选择,也可在播种过程中用本发明活性物质组合物处理种子。
在本发明种子或土壤处理的另一实施方案中,将合适的话呈含水悬浮液形式的本发明活性物质组合物引入已经含有种子的犁沟(furrow)中。作为选择,也可首先用本发明活性物质组合物或其含水制剂处理犁沟,然后将种子引入犁沟。
取决于所用活性物质的性质,本发明活性物质组合物适合于处理任何有用植物如禾谷类作物、根茎作物、油料作物、蔬菜、香料作物、观赏植物等的种子,例如适合于处理如下作物的种子:硬粒小麦和其它小麦类,燕麦,黑麦,大麦,玉米(饲料玉米和甜玉米),大豆,芸苔、棉花,向日葵,香蕉,稻,油菜,甜菜,糖用甜菜,饲料甜菜,茄子,土豆,草坪,草籽,西红柿,韭菜,南瓜,卷心菜,生菜植物、胡椒,黄瓜,甜瓜,菜豆,豌豆,大蒜,洋葱,胡萝卜,烟草,葡萄,矮牵牛,天竺葵,老鹳草,三色堇等。本发明活性物质组合物也适合于处理耐除草剂,如耐受磺酰脲类、咪唑啉酮类、草铵膦、草甘膦、环己二酮/芳氧基苯氧基丙酸除草剂的转基因作物的种子,以及适合处理适合于产生Bt毒素(苏云金芽孢杆菌(Bacillus thuringiensis)毒素)的种子。
本发明活性物质组合物优选以使得种子中活性物质的量为0.1g至10kg/100kg种子,优选1g至5kg/100kg种子,尤其是1g至2.5kg/100kg种子的量使用。对某些植物如生菜植物和洋葱而言,也可选择较大量的活性物质。
与常规处理的种子相比,已经根据本发明处理的种子有利特征显著且因此同样为本发明申请的主题。
作为选择,对已经生长的植物喷雾施用也是可行的。为此,可将本发明活性物质组合物直接以用水稀释形式或以稀释配制剂的形式直接施加至植物上。
本发明组合物也可掺入随后直接或以稀释形式,例如以含水喷雾混合物施用的活性物质配制剂中。这类配制剂可为固体、半固体,例如粉末、粉剂、糊、颗粒,或液体如悬浮液或分散体,如含水的、油基的或其它悬浮液或分散体。取决于所选配制剂,已经通过用水稀释获得的配制剂或喷雾混合物可通过喷雾、雾化、撒粉、撒播、浸泡或处理种子或与种子混合而施用。使用剂型取决于意欲目的;在任何情况下,它们应确保本发明活性物质的最佳可能分布。
除了本发明活性物质组合物之外,配制剂通常包含固体或液体载体和常用于植物保护产品的配制剂中的辅助剂。常用于植物保护产品的配制剂中的辅助剂的实例为表面活性物质(例如上述分散剂、保护胶体、乳化剂、润湿剂和粘合剂)和上述有机和无机增稠剂、杀菌剂、防冻剂、消泡剂,合适的话着色剂。
液体载体的实例为中到高沸点的矿物油馏分,如煤油或柴油,此外还有煤焦油和植物或动物源的油,脂族、环状和芳族烃,如石蜡、四氢萘、烷基化萘或其衍生物、烷基化苯或其衍生物,醇如甲醇、乙醇、丙醇、丁醇、环己醇或水。
固体载体为矿土如硅石、硅胶、硅酸盐、滑石、高岭土、石灰石、石灰、白垩、红玄武土、黄土、粘土、白云石、硅藻土、硫酸钙、硫酸镁、氧化镁,磨碎的合成材料,肥料如硫酸铵、磷酸铵、硝酸铵、脲类以及植物源的产品如谷粉、树皮粉、木粉和坚果壳粉,纤维素粉或其它固体载体。
如下实施例意欲说明本发明。
I.用于测定关于对硝基苯基乙酸酯水解的水解酶活性的分析
对硝基苯基乙酸酯以在二甲亚砜/异丙醇(1∶1V/V)中,浓度为5mg/ml的储备溶液的形式使用。
待试验脂肪酶以在0.1%BSA(牛血清蛋白)溶液中,浓度为1mg/ml的储备溶液使用。对试验而言,将该溶液用0.1%浓度BSA溶液稀释至酶浓度为0.001mg/ml。
试验在1.5ml Eppendorf容器中进行。在每种情况下,进行一个空白测定和三个重复测定。
为进行分析,将650μl去离子水,在0.1%BSA(0.001mg/ml)中的50μl脂肪酶,100μl MES缓冲剂(1M)和100μl对硝基苯基乙酸酯储备溶液放入Eppendorf容器中。
将容器在所需温度下,在水浴中放置2分钟。2分钟后,反应通过加入100μl 1M盐酸而终止。随后,通过HPLC测定所形成的硝基苯酚的量。
HPLC测定借助反向柱(reverse-phase column)(Merck HiBar RT250-4,Licrosorb RP18(5μm))进行。流速为1.00ml/分钟。注射体积为10.0μl。检测借助在280nm和326nm处的UV光谱法完成。所用洗脱液为在水中的0.1%三氟乙酸(洗脱液A)和在乙腈中的0.1%三氟乙酸(洗脱液B)的梯度。
II用于测定关于聚合物P的水解酶活性的分析
为此,将100mg的聚合物P和脂肪酶(1mg/ml)在22℃和110rpm下,在50ml磷酸二氢钾缓冲剂(5mM KH2PO4,pH 8)中震荡。在规律的间隔时间下测定pH值。一天后pH的显著变化表明聚合物被脂肪酶降解。
III制备本发明活性物质组合物:
原料:
聚己内酯:polymer P767E,购自Dow Plastics(数均分子量50000g/mol),
脂肪酶B,得自南极假丝酵母(Structure 1994,2,第293-298页)
戊叉唑菌(纯度>98%)
脂肪酶,得自伯克霍尔德氏菌(Burkholderia plantarii)(Burkholderiaglumae),如J.prakt.Chem.1997,339,第381-384页(Swiss-prot No.Q05489)中所述,
聚乙烯基吡咯烷酮:聚乙烯基吡咯烷酮粉末,K值约为17
(在水中的Fikentscher K值:Kollidon 17PF,购自BASFAktiengesellschaft)。
实施例1:
通过喷雾干燥制备本发明活性物质组合物
在合适的容器中,将10g聚己内酯、1.8g戊叉唑菌、0.7g南极假丝酵母脂肪酶和5g聚乙烯基吡咯烷酮粉末溶解在200g四氢呋喃中。在购自Büchi的实验室喷雾塔中将所得溶液喷雾至干燥气流中。干燥气体的入口温度为140℃,出口温度为80℃。以该方式获得初级粒度为1-100μm的粉末。
喷雾干燥后的残余活性借助在I.中所述的活性试验而测定。为此,将1mg/ml胶囊分散在0.1%浓度BSA水溶液中,且在经过一段时间之后,悬浮液的酶活性使用I.中所述试验测定。将所测活性转化为每克粉末的酶含量。
对比例2:
为检查包封效力,类似于实施例1,制备具有不同的聚己内酯和聚乙烯基吡咯烷酮含量的粉末(不含酶)。活性物质含量为10重量%。粉末具有1-100μm的初级粒度。
将所得粉末放入水中并在22℃下储存1小时。一小时后,取出胶囊,溶解在四氢呋喃中,借助UV-VIS测定残留在胶囊中的活性物质含量并将其与未处理的粉末样品的活性物质含量相比。结果显示在下表中。
实验 | PCL[重量%]1) | PVP[重量%]2) | 活性物质[%]3) |
A | 90 | 0 | 95 |
B | 75 | 25 | 70 |
C | 50 | 40 | 55 |
D | 30 | 60 | 12 |
1)聚己内酯,基于粉末的总重量
2)聚乙烯基吡咯烷酮,基于粉末的总重量
3)粉末中活性物质的残余量,基于新制粉末中100%活性物质
实施例3:测定活性物质的释放
由于酶在不同温度下具有不同活性,可将本发明组合物用于以温度依赖方式释放活性物质。参考如下实施例对其说明。
为此,类似于实施例1,制备具有如下组成的活性物质组合物:
66.7重量%聚己内酯,
19.3重量%聚乙烯基吡咯烷酮,
10重量%戊叉唑菌,和
4重量%伯克霍尔德氏菌(Burkholderia plantarii)(Burkholderiaglumae,Swiss-Prot No.Q 05489)脂肪酶。
使所得粉末(初级粒度为1-100μm)悬浮在水中并在5℃或22℃下储存1小时或6小时。在经过各自时间段之后,将胶囊分离,溶解在四氢呋喃中,借助UV/VIS测量而测定残余活性物质含量并将其与未处理样品的活性物质含量比较。结果显示在下表中。
1)粉末中残余的活性物质百分数,基于参考样品中100%活性物质。实施例4(应用实施例):
为了证实酶的存在影响释放,在对大豆仁研究由戊叉唑菌触发的枯萎,以及对萌发率的影响。
为此,类似于实施例1,制备具有如下组成的如下两种粉状活性物质组合物:
活性物质组合物4.1
29重量%聚己内酯,
58重量%聚乙烯基吡咯烷酮,
10重量%戊叉唑菌,和
3重量%伯克霍尔德氏菌(Burkholderia plantarii)(Burkholderiaglumae,Swiss-Prot No.Q 05489)脂肪酶。
活性物质组合物4.2(不是本发明的)
30重量%聚己内酯,
60重量%聚乙烯基吡咯烷酮,和
10重量%戊叉唑菌。
粉末具有0.1-10μm的初级粒度。
大豆仁cv.Lory用戊叉唑菌的市售FS配制剂和两种活性物质组合物4.1和4.2的水分散体分别处理。为此,在每种情况下分别以10和20g戊叉唑菌/100kg种子的施用率用样品处理50个大豆仁,并将大豆仁播种入充满沙的聚苯乙烯盘中。秧苗在18-22℃的温度和12小时光照下在温室中生长。播种27天后,对每个种子箱测定萌发率和平均植物高度。
应用实施例的结果
1)27DAT:测量在播种27天之后进行
从表1数据可以看出,在已经用含酶组合物处理过的植物中,枯萎比在不含酶的那些植物中更大。这表明由于酶,活性物质更快速地从胶囊中释放。同时,可以看到,由于包封,萌发率和植物高度比在常规FS配制剂中受影响程度小。
Claims (20)
1.一种呈细碎的含活性物质颗粒形式的活性物质组合物,该组合物包含:
a)至少一种植物保护剂;
b)至少一种不溶于水且可通过酶促水解降解的聚合物P,其量基于含活性物质颗粒的组分的总量为至少20重量%,和
c)至少一种水解酶(EC 3),
其中至少90重量%的活性物质组合物的含活性物质颗粒的直径不超过500μm(D90-值)且其中组分a)、b)和c)占活性物质颗粒的至少30重量%。
2.根据权利要求1的活性物质组合物,其中聚合物P在聚合物骨架上具有多个酯基且酶选自酯水解酶(EC 3.1)。
3.根据权利要求2的活性物质组合物,其中酶选自来自米曲霉(Aspergillus oryzae)的脂肪酶,来自腐皮镰孢(Fusarium solani)的角质酶和来自伯克霍尔德氏菌(Burkholderia plantarii)的脂肪酶和来自南极假丝酵母(Candida Antarctii)的脂肪酶。
4.根据权利要求2的活性物质组合物,其中聚合物P选自聚丙交酯、聚己内酯、聚丙交酯与聚乙二醇的嵌段共聚物以及聚己内酯与聚乙二醇的嵌段共聚物。
5.根据权利要求2的活性物质组合物,其中所述至少一种水解酶选自羧酸酯水解酶(EC 3.1.1),尤其是脂肪酶(EC 3.1.1.3)和角质酶(EC 3.1.1.74)。
6.根据前述权利要求中任一项的活性物质组合物,其中所述至少一种水解酶在低于10℃的温度下基本无活性。
7.根据前述权利要求中任一项的活性物质组合物,其中聚合物P具有大于40℃的玻璃化转变温度或熔点。
8.根据前述权利要求中任一项的活性物质组合物,其中在含活性物质颗粒中聚合物P以基于含活性物质颗粒的组分的总量为20-95重量%的量存在。
9.根据前述权利要求中任一项的活性物质组合物,其中所述至少一种活性物质选自具有杀真菌、杀虫、杀螨和/或杀线虫活性的有机化合物。
10.根据前述权利要求中任一项的活性物质组合物,其中在含活性物质颗粒中活性物质以基于含活性物质颗粒的组分的总量为5-30重量%的量存在。
11.根据前述权利要求中任一项的活性物质组合物,其包含至多70重量%的可在20℃下溶于水中的聚合物。
12.根据权利要求11的活性物质组合物,其中水溶性聚合物选自聚乙烯基吡咯烷酮、乙烯基吡咯烷酮/乙酸乙烯酯共聚物、聚乙烯基甲酰胺、部分水解的聚乙烯基甲酰胺、丙烯酸的均聚物和共聚物、甲基丙烯酸的均聚物和共聚物、丙烯酰胺的均聚物和共聚物、聚乙烯亚胺、聚乙烯胺、聚己内酰胺、聚乙烯醇、水解程度>50%的部分水解的聚乙酸乙烯酯、纤维素、纤维素衍生物、改性淀粉和淀粉衍生物、葡聚糖和聚C2-C3氧化烯。
13.一种制备根据前述权利要求中任一项的活性物质组合物的方法,其包括混合含活性物质颗粒的组分和进一步加工混合物以产生细碎粉末,其中在所述粉末中至少90重量%的活性物质组合物的含活性物质颗粒的直径不超过500μm(D90值)。
14.根据权利要求13的方法,其中活性物质组合物的制备包括将含活性物质颗粒的组分溶解或分散在合适的溶剂或稀释剂中并随后喷雾干燥所得分散体或溶液。
15.根据权利要求1-12中任一项的活性物质组合物在处理土壤中的用途。
16.根据权利要求1-12中任一项的活性物质组合物在处理植物中的用途。
17.根据权利要求1-12中任一项的活性物质组合物在处理种子中的用途。
18.包含根据权利要求1-12中任一项的活性物质组合物的种子。
19.一种含水组合物,包含分散在含水介质中的细碎的含活性物质颗粒形式的根据权利要求1-12中任一项的活性物质组合物。
20.一种制备根据权利要求18的含活性物质的种子的方法,其包括使常规种子与根据权利要求1-12中任一项的活性物质组合物或与根据权利要求19的含水组合物接触。
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AU751267B2 (en) * | 1997-06-30 | 2002-08-08 | Monsanto Technology Llc | Microparticles containing agricultural active ingredients |
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2008
- 2008-04-25 JP JP2010504715A patent/JP2010525031A/ja not_active Withdrawn
- 2008-04-25 US US12/597,113 patent/US20100122379A1/en not_active Abandoned
- 2008-04-25 CN CN200880021996A patent/CN101686664A/zh active Pending
- 2008-04-25 RU RU2009143556/21A patent/RU2009143556A/ru unknown
- 2008-04-25 BR BRPI0810552-9A2A patent/BRPI0810552A2/pt not_active Application Discontinuation
- 2008-04-25 EP EP08749754A patent/EP2150106A2/de not_active Ceased
- 2008-04-25 CA CA002683037A patent/CA2683037A1/en not_active Abandoned
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107347877A (zh) * | 2016-05-09 | 2017-11-17 | 中国科学院大学 | 一种含嵌段共聚物peg-pcl的朱砂叶螨抑制剂及其制备方法 |
CN107347877B (zh) * | 2016-05-09 | 2020-12-01 | 中国科学院大学 | 一种含嵌段共聚物peg-pcl的朱砂叶螨抑制剂及其制备方法 |
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US20100122379A1 (en) | 2010-05-13 |
WO2008132179A2 (de) | 2008-11-06 |
WO2008132179A3 (de) | 2009-04-30 |
RU2009143556A (ru) | 2011-06-10 |
CA2683037A1 (en) | 2008-11-06 |
EP2150106A2 (de) | 2010-02-10 |
JP2010525031A (ja) | 2010-07-22 |
BRPI0810552A2 (pt) | 2014-10-07 |
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