8%甲氰菊酯·丁氟螨酯纳米乳剂的研制及其性能

doi:10.3864/j.issn.0578-1752.2016.14.005

摘要/Abstract

摘要： 【目的】农药复配可扩大防治谱、降低单剂用药量和生产成本，延长药剂使用寿命。开发能耗低、稳定性好的纳米乳剂，使农药有效成分可以通过剂型加工更好地发挥其生物效果，提高药效。【方法】采用药膜法测定两种杀虫杀螨剂甲氰菊酯、丁氟螨酯对朱砂叶螨(Tetranychus cinnabarinus)的毒力，采用共毒因子法评价两个药剂的增效作用，共毒系数法进行复配农药最佳配比筛选，最后对配比与共毒系数进行数学模型方程拟合对最佳配比进行筛选；并在获得最佳配比的基础上采用低能乳化法加工成8%甲氰菊酯·丁氟螨酯纳米乳剂，根据联合国粮农组织纳米乳剂特性及基本要求，进行8%甲氰菊酯·丁氟螨酯纳米乳剂质量控制指标检测;并通过接触角和黏附功的测定初步探究纳米乳剂的性能。【结果】药膜法测定甲氰菊酯、丁氟螨酯处理朱砂叶螨雌成螨24 h后LC₅₀分别为711.62、4.32 mg·L^-1，共毒因子法测定结果表明，甲氰菊酯和丁氟螨酯复配在质量比18﹕1和165﹕1之间具有增效作用，增效配比区间较宽，两者复配可行。共毒系数法结果表明，甲氰菊酯与丁氟螨酯的质量比为50﹕1时，共毒系数（CTC）最高，CTC=209.96。通过方程拟合，甲氰菊酯·丁氟螨酯配比与共毒系数的数学模型为y=-216.86x²+19201x-424807，R²=0.864，理论最佳配比约为39﹕1（质量比），CTC=211.91，进一步通过共毒系数法对理论最佳配比验证得：甲氰菊酯﹕丁氟螨酯=39﹕1时，毒力回归方程为y=0.66x+3.8，r=0.9757，LC₅₀=60.96 mg·L^-1，共毒系数（CTC）高达215.36。由以上结果可知理论最佳配比与实际最佳配比增效作用基本一致，说明筛选的甲氰菊酯和丁氟螨酯最佳配比具有实际可靠性。最终确定39﹕1（甲氰菊酯﹕丁氟螨酯质量比）为最佳配比进行纳米乳剂的研制。通过溶剂、乳化剂、水质的筛选，得到8%甲氰菊酯·丁氟螨酯纳米乳剂的最佳制剂配方，优化配方为：甲氰菊酯7.8%，丁氟螨酯0.2%，溶剂10%（溶剂油S-150#﹕二甲苯=4﹕1），乳化剂9%—11%（十二烷基苯磺酸钙﹕聚氧乙烯脂肪酸酯=2﹕3），丙三醇2%，水补足至100%。所研制8%甲氰菊酯·丁氟螨酯纳米乳剂外观呈透明均相液体，乳液稳定性、低温稳定性、热贮稳定性、经时稳定性等指标均合格，稀释200倍呈淡蓝色均相透明液体且分散性良好。8%甲氰菊酯·丁氟螨酯纳米乳剂与两种单剂相比接触角更小，黏附功大，纳米乳液雾滴与靶标结合得更加牢固，药液不容易从靶标上洒落，更有利于植物对药液的吸收，可提高药效。【结论】采用共毒因子法、共毒系数法与拟合方程相结合进行最佳配比的筛选，其结果可以更全面、客观地反映出二元复配剂的增效情况，对农药复配有一定的指导价值，同时纳米乳剂的引入对于改善当前农药剂型结构具有重要意义。

关键词: 甲氰菊酯, 丁氟螨酯, 朱砂叶螨, 农药复配, 纳米乳剂, 接触角

Abstract: 【Objective】Pesticide mixtures can expand controlling spectrum, decrease pesticide dosage and the cost of production, and prolong the service life of insecticides. To a certain extent, nano-emulsion with low energy consumption and good stability can be developed. The effective components of the pesticide can produce biological effects better by pesticide formulation.【Method】Toxicities of fenpropathrin and cyflumetofen (two types of insecticide and acaricide) to Tetranychus cinnabarinus were determined by residual contact vial method. co-toxicity factor was used to evaluate the formulation synergism and co-toxicity coefficient method was adopted to screen the optimum ratio of pesticides, thus a mathematical model equation was fitted by using the method of optimum ratio and co-toxicity coefficient. Based on the optimum ratio, the 8% fenpropathrin·cyflumetofen nano-emulsion was processed by low-energy emulsification method. According to the characteristics of the nano-emulsion and the basic standards formulated by FAO, the quality control indexes of the product was developed. Finally, the performance of the nano-emulsion was primarily determined by the measurements of contact angle and adhesion work.【Result】After 24 h treatment, the LC₅₀ of fenpropathrin and cyflumetofen against T. cinnabarinus female adults was 711.62 and 4.32 mg·L^-1, respectively. Co-toxicity factors method showed that fenpropathrin and cyflumetofen complex had a synergistic effect. Results of the experiment showed that synergism was observed when the ratio of fenpropathrin to cyflumetofen was in range of 18﹕1 to 165﹕1. The synergetic ratio range of fenpropathrin to cyflumetofen is larger and it seems that this pesticide mixtures is feasible. Cotoxicity coefficient method showed the best synergistic effect of fenpropathrin﹕cyflumetofen was 50﹕1, co-toxicity coefficients was up to 209.96. The ratio mathematical model of fenpropathrin﹕cyflumetofen is y=-216.86x²+19201x-424807, R²=0.864, the optimum ratio in theory is 39﹕1, CTC=211.91. Through further cotoxicity coefficient and fitting equation analysis, it showed that toxicity regression equation is y=0.66x+3.8, r=0.9757, LC₅₀=60.96 mg·L^-1, the CTC value is 215.36 as the ratio of fenpropathrin to cyflumetofen was 39﹕1. Finally, this ratio of fenpropathrin to cyflumetofen (39﹕1) was selected as the optimum ratio for preparing nano-emulsion. Through optimization of solvent, emulsifier and water quality, the optimum formula is as follows: fenpropathrin 7.8%, cyflumetofen 0.2%, solvent 10% (ratio of 150# solvent naphtha﹕xylene=4﹕1), emulsifier 9%-11% (ratio of calciumalkylaromaticsulfonate﹕ polyoxyethylene aliphatate=2﹕3), propanetriol 2%, and water up to 100%. The 8% fenpropathrin·cyflumetofen nano-emulsion showed excellent performance, and the 100-fold dilution was pale blue homogeneous translucent liquid system with good dispersity. The experiment of contact angle showed that the 8% fenpropathrin·cyflumetofen nano-emulsion had the smaller contact angle and the 1arger adhesion work which was conducive to the absorption of plant leaves to liquid medicine and thus improve efficacy. 【Conclusion】 Optimal proportions was screened by means of co-toxicity factor, cotoxicity coefficient and fitting equation, which can be more comprehensively and objectively reflect the efficiency of the two compound agents, as well as to provide certain references for pesticide mixtures. It will provide some instructive significance to combined pesticides.

Key words: fenpropathrin, cyflumetofen, Tetranychus cinnabarinus, pesticide mixtures, nano-emulsion, contact angle

赵恒科，蓝月，南灿，胡月，饶萍，田亚，严伟，钱坤，何林. 8%甲氰菊酯·丁氟螨酯纳米乳剂的研制及其性能[J]. 中国农业科学, 2016, 49(14): 2700-2710.

ZHAO Heng-ke, LAN Yue, NAN Can, HU Yue, RAO Ping, TIAN Ya, YAN Wei, QIAN Kun, HE Lin. Preparation of 8% Fenpropathrin·Cyflumetofen Nano-Emulsion and Its Performance[J]. Scientia Agricultura Sinica, 2016, 49(14): 2700-2710.

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