溶剂蒸发法制备丙硫菌唑微囊及其性能研究

doi:10.3864/j.issn.0578-1752.2021.04.008

Abstract

Abstract:

【Objective】The biodegradable material poly (3-hydroxybutyrate-co-4-hydroxybutyrate) (P (3HB-co-4HB)) was used as the wall material to prepare prothioconazole microcapsules. The effect of preparation process on the microcapsule size, pesticide loading and encapsulation efficiency was optimized. The microcapsules with good dispersion, small particle size, and high pesticide loading were screened out, and the preliminary researches on the release kinetics, photodegradation, and indoor biological activity on Sclerotium rolfsii were carried out. The purpose of this study is to provide a theoretical basis and technical support for improving the stability and utilization efficiency of prothioconazole in the environment.【Method】The solvent evaporation method was used to prepare prothioconazole microcapsules, and the effects of the mass ratio of core to wall material, volume ratio of oil to water, mass fraction of emulsifier and shearing speed on the particle size, pesticide loading and encapsulation efficiency of the microcapsules were investigated through a single factor test. Taking pesticide loading and particle size as the key technical indicators, the optimal preparation parameters were screened out through the L₉(3⁴) orthogonal test, which was further verified. The morphological and structural features, release performance and photodegradability of the microcapsules were determined by scanning electron microscope (SEM), fourier transform infrared (FTIR) spectrometer, and high performance liquid chromatography (HPLC). The toxicity of prothioconazole microcapsules on S. rolfsii was investigated by indoor bioassay.【Result】The mass ratio of core to wall material had a significant effect on the pesticide loading capacity of the microcapsules. As the ratio of core material increased, the loading capacity gradually increased. The volume ratio of oil to water, PVA mass fraction, and shearing speed had significant effects on the microcapsule particle size. As the shearing speed and PVA mass fraction increased, the microcapsule particle size gradually decreased. The volume ratio of oil to water had a great influence on the morphology and dispersion of microcapsules, and the influence of various factors on the encapsulation efficiency of the microcapsules was not significant. The optimal preparation parameters obtained through the L₉(3⁴) orthogonal test was as follows: the mass ratio of core to wall material of 1﹕5, volume ratio of oil to water of 1﹕5, PVA mass fraction of 2%, and shearing speed of 12 000 r/min. Under the optimal preparation process, spherical prothioconazole microcapsules with a particle size (D₅₀) of 3.32 μm and a span of 2.82 were prepared with a loading content of 15.52% and an encapsulation efficiency of 80.24%. Compared with prothioconazole technical material, the microcapsules had better sustained-release performance, and the release kinetics conformed to Fick’s diffusion law, presenting two processes of “burst release” followed by “sustained release”. The photostability of prothioconazole in the microcapsules in aqueous solution was enhanced, and the half-life of photolysis was doubled. The mycelial growth rate inhibition result showed that the fungicidal activity of prothioconazole microcapsules against S. rolfsii was equivalent to that of prothioconazole technical material.【Conclusion】Prothioconazole microcapsules with biodegradable material P (3HB-co-4HB) as a carrier were prepared, and different preparation processes affect the pesticide loading, dispersion state and particle size of microcapsules. The slow and sustained release and photostability are of great significance for reducing the amount of pesticide applied and improving the utilization efficiency of pesticide, which has potential application in control of peanut southern blight.

Key words: prothioconazole, polyhydroxybutyrate, microcapsule, preparation process, controlled release, Sclerotium rolfsii

CHEN Ge,CAO LiDong,XU ChunLi,ZHAO PengYue,CAO Chong,LI FengMin,HUANG QiLiang. Performance Study of Prothioconazole Microcapsules Prepared by Solvent Evaporation Method[J].Scientia Agricultura Sinica, 2021, 54(4): 754-767.

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References 51

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因素水平 Factor level	1	2	3	4
芯壁材质量比 Mass ratio of core to wall material	1﹕5	1﹕10	1﹕20
油水体积比 Volume ratio of oil to water	1﹕5	1﹕10	1﹕15	1﹕20
PVA质量分数 Mass fraction of PVA (%)	0.5	1	1.5	2
剪切速率 Shearing speed (r/min)	4000	8000	12000

水平 Level	因素Factor
水平 Level	A	B	C	D
1	1﹕15	1﹕15	0.5%	4000
2	1﹕10	1﹕10	1%	8000
3	1﹕5	1﹕5	2%	12000

PVA质量分数 Mass fraction of PVA (%)	载药量 Loading content (%)	包封率 Encapsulation efficiency (%)	粒径 D₅₀ (μm)	跨距 Span
0.5	15.58±0.83a	77.47±5.79a	4.61±0.06a	3.70b
1	15.69±0.21a	78.90±1.47a	3.46±0.06b	4.26a
1.5	15.67±0.34a	80.47±4.07a	3.21±0.06c	3.69b
2	15.12±1.69a	78.70±3.04a	2.55±0.04d	2.91c

芯壁质量比 Mass ratio of core to wall	载药量 Loading content (%)	包封率 Encapsulation efficiency (%)	粒径 D₅₀(μm)	跨距 Span
1﹕5	15.31±2.28a	77.04±7.26a	3.46±0.06b	4.26a
1﹕10	7.69±0.98b	75.99±2.10a	3.47±0.05b	4.08b
1﹕20	4.66±0.12c	71.72±2.92a	4.33±0.08a	4.22a

油水体积比 Volume ratio of oil to water	载药量 Loading content (%)	包封率 Encapsulation efficiency (%)	粒径 D₅₀(μm)	跨距 Span
1﹕5	15.38±1.34a	76.98±6.36a	3.46±0.06a	4.26c
1﹕10	15.35±0.34a	67.07±6.39a	2.65±0.01d	4.52b
1﹕15	14.82±2.36a	68.08±6.53a	3.13±0.03b	4.29c
1﹕20	14.88±1.09a	74.26±4.34a	2.90±0.08c	5.38a

Performance Study of Prothioconazole Microcapsules Prepared by Solvent Evaporation Method

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乳化剪切速率 Shearing speed (r/min)	载药量 Loading content (%)	包封率 Encapsulation efficiency (%)	粒径 D₅₀(μm)	跨距 Span
4000	15.29±0.76a	78.31±1.51a	12.61±2.26a	3.54b
8000	15.34±1.35a	77.88±3.02a	3.46±0.05b	4.26a
12000	15.84±0.38a	78.33±2.54a	2.06±0.06c	2.87c

试验编号 Trial number	A	B	C	D	载药量 Loading content (%)	粒径 D₅₀ (μm)
1	1	1	1	1	5.43	15.50
2	1	2	2	2	4.03	4.06
3	1	3	3	3	5.53	2.15
4	2	1	2	3	7.76	2.62
5	2	2	3	1	8.00	10.69
6	2	3	1	2	9.64	4.33
7	3	1	3	2	14.68	2.62
8	3	2	1	3	13.86	2.20
9	3	3	2	1	15.94	12.61

极差分析 Range analysis		因素Factor
极差分析 Range analysis		A	B	C	D
载药量 Loading content (%)	K₁	5.00	9.29	9.64	9.79
	K₂	8.47	8.63	9.24	9.45
	K₃	14.83	10.37	9.40	9.05
	R	9.83	1.74	0.40	0.74
粒径 Particle size (μm)	K₁	7.24	6.91	7.34	12.93
	K₂	5.88	5.65	2.96	3.67
	K₃	5.81	6.36	5.15	2.32
	R	1.43	1.27	4.39	10.61

	拟合模型 Fitting model	动力学方程 Kinetic equation (Q=)	决定系数 Determination coefficient (R²)
原药TC	零级拟合Zero-order fitting	0.23t+ 28.21	0.5015
	一级拟合First-order fitting	46.22 (1-e^-0.14t)	0.9727
	Higuchi拟合Higuchi fitting	3.20t^1/2+19.33	0.6789
	Ritger-Peppas 拟合Ritger-Peppas fitting	18.40t^0.22	0.8000
微囊MC	零级拟合Zero-order fitting	0.55t+22.05	0.9159
	一级拟合First-order fitting	72.31(1-e^-0.04t)	0.8501
	Higuchi拟合Higuchi fitting	6.94t^1/2+5.63	0.9596
	Ritger-Peppas 拟合Ritger-Peppas fitting	10.65t^0.42	0.9622

丙硫菌唑 Prothioconazole	一级动力学方程 First-order kinetic equation			T_1/2 (h)
丙硫菌唑 Prothioconazole	C_t=C₀e^-kt	k (min^-1)	R²	T_1/2 (h)
微囊MC	y=54.04e^-0.0076t	0.0076	0.975	1.52
原药TC	y=54.57e^-0.0151t	0.0151	0.997	0.76

样品 Sample	浓度 Concentration (mg·L^-1)	菌落直径 Colony diameter (cm)	抑制率 Inhibition rate (%)
CK	—	7.95	—
丙硫菌唑原药 Prothioconazole TC	2.5	4.47	46.09±2.19
	5.0	3.89	53.77±1.89
	10.0	3.24	62.38±4.56
	20.0	2.37	73.91±8.43
	40.0	0.80	94.70±1.30
丙硫菌唑微囊 Prothioconazole MC （DMSO溶解 Dissolved with DMSO）	2.5	4.24	49.14±6.94
	5.0	3.83	54.57±9.46
	10.0	3.52	58.68±5.61
	20.0	1.99	78.94±6.25
	40.0	0.93	92.98±1.82
丙硫菌唑微囊 Prothioconazole MC （无菌水分散 Dispersal in sterile water）	2.5	4.53	48.89±1.17
	5.0	4.12	53.96±2.60
	10.0	3.39	63.00±3.51
	20.0	3.04	67.32±2.88
	40.0	2.40	75.25±4.65

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