正交设计和均匀设计在优化噻虫胺悬浮剂物理稳定性上的应用  

Application of Orthogonal Design and Uniform Design in Physical Stability Promotion of Clothianidin Suspension Concentrate

作　　者：李北兴[1] 王伟昌[1] 张大侠[1] 王凯[1] 管磊[1] 刘峰[1] 

机构地区：[1]山东农业大学植物保护学院/农药毒理与应用技术重点实验室,山东泰安271018

出　　处：《中国农业科学》2015年第2期280-292,共13页Scientia Agricultura Sinica

基　　金：国家公益性行业(农业)科研专项(201303027)

摘　　要：【目的】比较正交和均匀设计两种多因素试验方法在水悬浮剂配方中应用的优缺点,为该方法在农药制剂学领域的应用提供参考。【方法】在采用流点法初筛得到润湿性能良好的润湿分散剂之后,分别采用正交设计和均匀设计制备30%噻虫胺悬浮剂。综合考察润湿分散剂和黏度调节剂对制剂热贮析水率、离心沉淀率、黏度、流动性、分散性、热贮前后样品的粒度分布(D10、D50和D90)和悬浮率的影响。通过主效应图分析正交试验结果,采用逐步回归和偏最小二乘法(PLS)分析均匀试验结果,最后检验优化配方的各项性能。【结果】正交试验和均匀试验的所有样品黏度均在144.50—317.84 m Pa·s,均具有良好(良级或优级)的流动性和分散性。由于奥氏熟化作用,样品经热贮后,粒子的粒径轻微增大,D10、D50和D90分别由0.56—1.00、0.88—1.53和1.77—2.68μm变为0.76—1.02、1.12—1.56和2.07—3.25μm。所有样品贮前悬浮率均在91.88%—96.39%,经热贮后样品的悬浮率变化不大,分别在91.91%—96.13%,符合悬浮剂质量控制的一般要求,故本研究主要优化了热贮析水率和离心沉淀率两个指标。正交试验分析结果表明,T2700、黄原胶和硅酸镁铝的用量对热贮析水率和离心沉淀率均有显著影响,且均随用量增加而降低,而NR1601的用量对两个因变量的影响不显著。采用正交设计优化的配方,样品黏度为229.6 m Pa·s,流动性和分散性良好,热贮前后悬浮率分别为(94.76±0.70)%和(93.50±0.20)%,热贮析水率为(4.23±0.19)%,离心沉淀率也低于10%。均匀设计中,PLS平方项模型对热贮析水率有良好的预测性,热贮析水率为(2.55±0.03)%,离心沉淀率也仅为(4.36±0.21)%,优化样品的黏度为324.16 m Pa·s,流动性和分散性良好,热贮前后悬浮率分别为(93.19±0.09)%和(92.77±0.22)%,粒子的粒径小且分布较窄。PLS线性模型对离心沉淀率表现出良好的预测性,�[Objective] The objective of this study is to discuss the advantages and disadvantages in application of two multi-factor experimental designs in SC （suspension concentrate） formula. Effectively providing reference for the application of orthogonal design and uniform design in pesticide formulation was also expected. [Method] Clothianidin 30% SC was prepared based on orthogonal design and uniform design after the wetting-suspending agents with favorable wettability were selected by applying flow point method. The effect of wetting-suspending agent and viscosity modifier on the water separation rate after hot storage （WSRHS）, precipitation rate after centrifugation （PRC）, viscosity, fluidity, dispersibility, the size distribution （including Dl0, D50 and D90 and suspensibility of the samples before and after hot storage were investigated. The main effect plots were used to analyze the results of orthogonal design while stepwise regression and partial least squares （PLS） were used to analyze that of uniform design. Finally, validation tests were conducted to assess the properties of optimized formulas. [Result] The viscosity of all samples prepared based on orthogonal design and uniform design ranged from 144.50 to 317.84 mPa.s and all the samples exhibited favorable fluidity and dispersibility. Particle size became larger after hot storage due to ostwald ripening. The D10, D50and D90 were 0.56-1.00, 0.88-1.53 and 1.77-2.68 pm for samples before storage and 0.76-1.02, 1.12-1.56 and 2.07-3.25 p.m for samples after hot storage, respectively. Little change was observed for the suspensibility even after hot storage, of which the suspensibility ranged from 91.88% to 96.39% before storage and 91.91% to 96.13% after hot storage. Given the favorable performance the authors had measured which could satisfy the general requirements of SC quality control, only WSRHS and PRC were mainly optimized in this study. The ANOVA （analysis of variance） results of orthogonal design indicated that the dosage of T2700

关 键 词：正交设计 均匀设计 偏最小二乘法 逐步回归 物理稳定性 

分 类 号：TQ450.1[化学工程—农药化工]