固体增溶/分散技术制备啶虫脒可溶粒剂
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摘要
为了实现对难溶或微溶农药的高效利用,并满足速效、低毒和绿色环保的要求,采用医药研究中常用的固体增溶/分散技术,以聚乙二醇10000为固体增溶/分散介质,TANEMULCON1为分散剂,氯化铵为崩解剂,经混合造粒制备了啶虫脒可溶粒剂。当配方(以质量分数计)为啶虫脒30%、PEG10000 60%、分散剂TANEMULCON1 4%、氯化铵补足至100%时,啶虫脒可溶粒剂具有性质稳定、崩解速率快、能形成稳定的真溶液的特性。表明固体增溶/分散技术是将难溶于水的农药制备成可溶粒剂的一种简单、优良的新方法。
To enhance the utilization ratio of water-insoluble or sparingly soluble pesticides,and meet the requirements of fast-action,low toxicity as well as environment protection,solid solubilization/dispersion technology was explored for preparing soluble granules from water-insoluble or sparingly soluble pesticides.It was possible to prepare soluble granules with acetamiprid when polyethylene glycol 10000,TANEMULCON1 and ammonia chloride were used as solid solubilizing/dispersion carrier,dispersant and disintegrant,respectively.The optimized formula in weight percentage was acetamiprid 30%,polyethylene glycol 10000 60%,TANEMULCON1 4%,and ammonia chloride of the others.It was showed that the acetamiprid soluble granule of optimized formula was stable for storage,fast disintegration and available to form stable true solution in water.The results suggest that solid solubilization/dispersion technology is a simple,excellent tool for prepareing water soluble granules from insoluble pesticides technical meterials.
To enhance the utilization ratio of water-insoluble or sparingly soluble pesticides,and meet the requirements of fast-action,low toxicity as well as environment protection,solid solubilization/dispersion technology was explored for preparing soluble granules from water-insoluble or sparingly soluble pesticides.It was possible to prepare soluble granules with acetamiprid when polyethylene glycol 10000,TANEMULCON1 and ammonia chloride were used as solid solubilizing/dispersion carrier,dispersant and disintegrant,respectively.The optimized formula in weight percentage was acetamiprid 30%,polyethylene glycol 10000 60%,TANEMULCON1 4%,and ammonia chloride of the others.It was showed that the acetamiprid soluble granule of optimized formula was stable for storage,fast disintegration and available to form stable true solution in water.The results suggest that solid solubilization/dispersion technology is a simple,excellent tool for prepareing water soluble granules from insoluble pesticides technical meterials.
引文
[1]江苏瑞禾化学有限公司.啶虫脒水分散粒剂及其制备方法:中国CN 101258849[P].2008-09-10.Jiangsu Ruihe Chemical Company Limited.The acetamipridwater dispersible granules and its preparation method:CN101258849[P].2008-09-10.(in Chinese)
[2]庾琴,周华,王静,等.啶虫脒在环境中的降解代谢及其安全性的研究进展[J].农药,2007,46(4):223-226.YU Qin,ZHOU Hua,WANG Jing,et al.Methods researchprogress on degradation of acetamiprid and safety to environment[J].Agrochemicals,2007,46(4):223-226.(in Chinese)
[3]邓业成,王萌长,李洁荣,等.啶虫脒的杀虫活性研究[J].西南农业学报,2002,15(1):50-53.DENG Yecheng,WANG Mengchang,LI Jierong,et al.A studyon the insecticidal activity of acetaniprid on insects[J].SouthwestChina J Agric Sci,2002,15(1):50-53.(in Chinese)
[4]明亮,娄远来.国内外农药剂型研究进展及发展方向[J].江苏农业科学,2007(6):102-105.MING Liang,LOU Yuanlai.Developing direction and researchingprogress of pesticide formulation at home and abroad[J].JiangsuAgric Sci,2007(6):102-105.(in Chinese)
[5]张荣胜.8种登记含量的啶虫脒水分散粒剂配方研究[R].青岛:第九届山东省农药信息交流会,2009.ZHANG Rongsheng.Study on 8 registered formulation ofacetamiprid water dispersible granule[R].Qingdao:The NinthShangdong Province Pesticide Information Exchange,2009.(inChinese)
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[7]刘步林.农药剂型加工技术[M].北京:化学工业出版社,1998:198-217.LIU Bulin.Pesticide Formulation and Processing Technologies[M].Beijing:Chemical Industry Press,1998:198-217.(inChinese)
[8]栾贵书.溴虫腈水溶性粒剂及其制备方法[P].中国CN10156825[P].2009-10-28.LUAN Guishu.Chlorfenapyr water soluble granule and itspreparation method:CN 10156825[P].2009-10-28.(inChinese)
[9]戴宝江,吴明,任新峰.50%烯啶虫胺水溶粒剂的配方及应用研究[J].现代农药,2007.6(6):15-16.DAI Baojiang,WU Ming,REN Xinfeng.Study on theformulation and application of nitenpyram 50%WSG[J].Modern Agrochemicals,2007,6(6):15-16.(in Chinese)
[10]张惠平,向大雄,罗杰英等.固体分散技术在药剂学中的研究进展[J].中国药学杂志,2007,42(11):807-809.ZHANG Huiping,XIANG Da qiong,LUO Jieying,et al.Thedevelopment of solid dispersion techniques in pharmaceutics[J].Chinese Pharmac J,2007,42(11):807-809.(in Chinese)
[11]沈松,徐希明,余江南.难溶性药物的增溶及其缓/控释制剂研究进展[J].中国药事,2007,21(3):196-200.SHEN Song,XU Ximing,YU Jiangnan.Solubilization of poolysoluble drugs and research progress in slow/controlled releaseformulations[J].Chinese Pharmaceutical Affairs,2007,21(3):196-200.(in Chinese)
[12]马琳怡,韩丽妹,张志荣,等.银杏内酯固体分散体的制备和体外特性研究[J].中国中药杂志,2009,34(11):1368-1372.MA Linyi,HAN Limei,ZHANG Zhirong,et al.Preparation andcharacterization of solid dispersions of ginkgolides[J].China JChinese Mat Med,2009,34(11):1368-1372.(in Chinese)
[13]林辉,汪萌,邹慧琴,等.固体分散技术的研究进展[J].中国民间疗法,2012,20(8):78-79.LIN Hui,WANG Meng,ZOU Huiqin,et al.The researchprogress of solid dispersion[J].China's Naturopathy,2012,20(8):78-79.(in Chinese)
[14]陈周全,张宁.固体分散体技术在中药制剂中的应用概况[J].中国药房,2012.23(15):1427-1429.CHEN Zhouquan,ZHANG Ning.An overview about theapplication of solid dispersion in traditional Chinese medicine[J].China Pharmacy,2012,23(15):1427-1429.(in Chinese)
[15]林瑞来.难溶性药物溶解度的提高方法[J].中国医药指南,2010,8(3):33-34.LIN Ruilai.Methods to improve the solubility of insoluble drugs[J].Guide of China Medicine,2010,8(3):33-34.(in Chinese)
[16]孙建绪,王东兴.固体分散技术在药物制剂学研究中的应用[J].首都医药,2003(20):17-19.SUN Jianxu,WANG Dongxing.The appilcation of soliddipersion technology in pharmaceutical engineering[J].CapitalMedicine,2003(20):17-19.(in Chinese)
[17]周海云,陈钧,陆琪.青黛脂溶性提取物固体分散体制备及溶解性研究[J].时珍国医国药,2007,18(11):2756-2758.ZHOU Haiyun,CHEN Jun,LU Qi.Preparation and solubilitycharacterization of lipophilic indigo extracts solid dispersions[J].Lishizhen Medicine and Mat Med Res,2007,18(11):2756-2758.(in Chinese)
[18]HG/T2467.16—2003,农药可溶粒剂产品标准编写规范[S].沈阳,2004.5:56-56.HG/T2467.16—2003,Specification guidelines for pesticidesoluble granules[S].Shenyang,2004.5:56-56.(in Chinese)
[19]冯彤英,矫庆泽,张强,等.75%噻吩磺隆WG的配方研究与应用[J].农药,2006,45(9):603-605.FENG Tongying,JIAO Qingze,ZHANG Qiang,et al.Formulation and utilization of a thifensulfuron 75%waterdispersible granule[J].Agrochemicals,2006,45(9):603-605.(in Chinese)
[20]GB/T1600—1993,农药pH值的测定方法[S].北京.1993.GB/T1600—1993,Determination method of pH value forpesticides[S].Beijing,1993.(in Chinese)
[21]GB/T28137—2011,农药持久起泡性测定方法[S].浙江,2011.GB/T 28137—2011,Testing method of persistent foaming forpesticides[S].Zhejiang,2011.(in Chinese)
[22]HG/T2467.15—2003,农药可溶粉剂产品标准编写规范[S].沈阳,2004.5:55-56.HG/T2467.15—2003,Specification guidelines for solublepowder[S].Shenyang,2004.5:55-56.(in Chinese)
[23]GB/T607—1977,水分测定法[S].上海,1977.GB/T607—1977,Determinating the moisture content[S].Shanghai,1977.(in Chinese)
[24]宋永婷.水分散粒剂和水溶性粒剂农药研究[D].重庆:重庆大学,2012.Song Yongting.Research on pesticides of water dispersible andwater soluble granules[D].Chongqing:Chongqing University,2012.
[25]GB13200—91,水质浊度的测定[S].北京,1991.GB13200—91,Water quality-Determination of turbidity[S].Beijing,1991.(in Chinese)
[2]庾琴,周华,王静,等.啶虫脒在环境中的降解代谢及其安全性的研究进展[J].农药,2007,46(4):223-226.YU Qin,ZHOU Hua,WANG Jing,et al.Methods researchprogress on degradation of acetamiprid and safety to environment[J].Agrochemicals,2007,46(4):223-226.(in Chinese)
[3]邓业成,王萌长,李洁荣,等.啶虫脒的杀虫活性研究[J].西南农业学报,2002,15(1):50-53.DENG Yecheng,WANG Mengchang,LI Jierong,et al.A studyon the insecticidal activity of acetaniprid on insects[J].SouthwestChina J Agric Sci,2002,15(1):50-53.(in Chinese)
[4]明亮,娄远来.国内外农药剂型研究进展及发展方向[J].江苏农业科学,2007(6):102-105.MING Liang,LOU Yuanlai.Developing direction and researchingprogress of pesticide formulation at home and abroad[J].JiangsuAgric Sci,2007(6):102-105.(in Chinese)
[5]张荣胜.8种登记含量的啶虫脒水分散粒剂配方研究[R].青岛:第九届山东省农药信息交流会,2009.ZHANG Rongsheng.Study on 8 registered formulation ofacetamiprid water dispersible granule[R].Qingdao:The NinthShangdong Province Pesticide Information Exchange,2009.(inChinese)
[6]中国农药信息网.通过有效成分查询产品[DB/OL][2013-07-01].http:∥www.chinapesticide.gov.cn/service/aspx/B3X.aspx?aiid=ARACMChina Pesticide Information Network[DB/OL][2013-07-01].http:∥www.chinapesticide.gov.cn/service/aspx/B3X.aspx?aiid=ARACM(in Chinese)
[7]刘步林.农药剂型加工技术[M].北京:化学工业出版社,1998:198-217.LIU Bulin.Pesticide Formulation and Processing Technologies[M].Beijing:Chemical Industry Press,1998:198-217.(inChinese)
[8]栾贵书.溴虫腈水溶性粒剂及其制备方法[P].中国CN10156825[P].2009-10-28.LUAN Guishu.Chlorfenapyr water soluble granule and itspreparation method:CN 10156825[P].2009-10-28.(inChinese)
[9]戴宝江,吴明,任新峰.50%烯啶虫胺水溶粒剂的配方及应用研究[J].现代农药,2007.6(6):15-16.DAI Baojiang,WU Ming,REN Xinfeng.Study on theformulation and application of nitenpyram 50%WSG[J].Modern Agrochemicals,2007,6(6):15-16.(in Chinese)
[10]张惠平,向大雄,罗杰英等.固体分散技术在药剂学中的研究进展[J].中国药学杂志,2007,42(11):807-809.ZHANG Huiping,XIANG Da qiong,LUO Jieying,et al.Thedevelopment of solid dispersion techniques in pharmaceutics[J].Chinese Pharmac J,2007,42(11):807-809.(in Chinese)
[11]沈松,徐希明,余江南.难溶性药物的增溶及其缓/控释制剂研究进展[J].中国药事,2007,21(3):196-200.SHEN Song,XU Ximing,YU Jiangnan.Solubilization of poolysoluble drugs and research progress in slow/controlled releaseformulations[J].Chinese Pharmaceutical Affairs,2007,21(3):196-200.(in Chinese)
[12]马琳怡,韩丽妹,张志荣,等.银杏内酯固体分散体的制备和体外特性研究[J].中国中药杂志,2009,34(11):1368-1372.MA Linyi,HAN Limei,ZHANG Zhirong,et al.Preparation andcharacterization of solid dispersions of ginkgolides[J].China JChinese Mat Med,2009,34(11):1368-1372.(in Chinese)
[13]林辉,汪萌,邹慧琴,等.固体分散技术的研究进展[J].中国民间疗法,2012,20(8):78-79.LIN Hui,WANG Meng,ZOU Huiqin,et al.The researchprogress of solid dispersion[J].China's Naturopathy,2012,20(8):78-79.(in Chinese)
[14]陈周全,张宁.固体分散体技术在中药制剂中的应用概况[J].中国药房,2012.23(15):1427-1429.CHEN Zhouquan,ZHANG Ning.An overview about theapplication of solid dispersion in traditional Chinese medicine[J].China Pharmacy,2012,23(15):1427-1429.(in Chinese)
[15]林瑞来.难溶性药物溶解度的提高方法[J].中国医药指南,2010,8(3):33-34.LIN Ruilai.Methods to improve the solubility of insoluble drugs[J].Guide of China Medicine,2010,8(3):33-34.(in Chinese)
[16]孙建绪,王东兴.固体分散技术在药物制剂学研究中的应用[J].首都医药,2003(20):17-19.SUN Jianxu,WANG Dongxing.The appilcation of soliddipersion technology in pharmaceutical engineering[J].CapitalMedicine,2003(20):17-19.(in Chinese)
[17]周海云,陈钧,陆琪.青黛脂溶性提取物固体分散体制备及溶解性研究[J].时珍国医国药,2007,18(11):2756-2758.ZHOU Haiyun,CHEN Jun,LU Qi.Preparation and solubilitycharacterization of lipophilic indigo extracts solid dispersions[J].Lishizhen Medicine and Mat Med Res,2007,18(11):2756-2758.(in Chinese)
[18]HG/T2467.16—2003,农药可溶粒剂产品标准编写规范[S].沈阳,2004.5:56-56.HG/T2467.16—2003,Specification guidelines for pesticidesoluble granules[S].Shenyang,2004.5:56-56.(in Chinese)
[19]冯彤英,矫庆泽,张强,等.75%噻吩磺隆WG的配方研究与应用[J].农药,2006,45(9):603-605.FENG Tongying,JIAO Qingze,ZHANG Qiang,et al.Formulation and utilization of a thifensulfuron 75%waterdispersible granule[J].Agrochemicals,2006,45(9):603-605.(in Chinese)
[20]GB/T1600—1993,农药pH值的测定方法[S].北京.1993.GB/T1600—1993,Determination method of pH value forpesticides[S].Beijing,1993.(in Chinese)
[21]GB/T28137—2011,农药持久起泡性测定方法[S].浙江,2011.GB/T 28137—2011,Testing method of persistent foaming forpesticides[S].Zhejiang,2011.(in Chinese)
[22]HG/T2467.15—2003,农药可溶粉剂产品标准编写规范[S].沈阳,2004.5:55-56.HG/T2467.15—2003,Specification guidelines for solublepowder[S].Shenyang,2004.5:55-56.(in Chinese)
[23]GB/T607—1977,水分测定法[S].上海,1977.GB/T607—1977,Determinating the moisture content[S].Shanghai,1977.(in Chinese)
[24]宋永婷.水分散粒剂和水溶性粒剂农药研究[D].重庆:重庆大学,2012.Song Yongting.Research on pesticides of water dispersible andwater soluble granules[D].Chongqing:Chongqing University,2012.
[25]GB13200—91,水质浊度的测定[S].北京,1991.GB13200—91,Water quality-Determination of turbidity[S].Beijing,1991.(in Chinese)