20%异丙甲 • 苄泡腾片剂的研制及其对稻田杂草的防治效果

延卫垚; 杨景涵; 马英剑; 秦敦忠; 陈旺; 陈志洋; 冯建国

doi:10.16801/j.issn.1008-7303.2022.0010

20%异丙甲 • 苄泡腾片剂的研制及其对稻田杂草的防治效果

doi: 10.16801/j.issn.1008-7303.2022.0010

1.
扬州大学园艺与植物保护学院，江苏扬州 225009
2.
江苏擎宇化工科技有限公司，江苏扬州 211400

基金项目: 江苏省大学生创新创业训练计划(202011117049Z)；江苏省研究生科研与实践创新计划项目(SJCX21_1613).

详细信息

作者简介:
延卫垚，2798970967@qq.com

通讯作者:
冯建国，jgfeng@yzu.edu.cn.

中图分类号: TQ450.6
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- 文章访问数: 66
- HTML全文浏览量: 22
- PDF下载量: 7
- 被引次数: 0
出版历程
- 收稿日期: 2021-01-22
- 录用日期: 2021-12-07
- 网络出版日期: 2022-02-09

Preparation of metolachlor + bensulfuron-methyl 20% effervescent tablets and its control efficacy on weeds in paddy field

1.
School of Horticulture and Plant Protection, Yangzhou University, Yangzhou 225009, Jiangsu Province, China
2.
Jiangsu Sinvochem S&T Co., Ltd., Yangzhou 211400, Jiangsu Province, China

Funds: the Innovation and Entrepreneurship Training Program for College Students in Jiangsu Province (202011117049Z), The Postgraduate Research &Practice Innovation Program of Jiangsu Province(SJCX21_1613).

摘要

摘要: 为了提高稻田杂草化学防除的省力化程度，降低防治成本，通过单一变量法筛选配方中的助剂种类和用量，采用干法压片工艺制备了20%异丙甲 • 苄泡腾片剂 (有效成分异丙甲草胺 + 苄嘧磺隆)，同时进行了田间药效评价。结果表明：20%异丙甲 • 苄泡腾片剂的优化配方(质量分数)为：16%异丙甲草胺，4%苄嘧磺隆，18%有机膨润土，9%白炭黑，20%酒石酸，20%碳酸氢钠，6%润湿剂EFW，4%分散剂G202和3%润滑剂硬脂酸镁。该泡腾片剂在有效成分120~180 g/hm² 的用量范围内能有效防除稻田杂草，防效明显优于其单剂，与已登记的20%异丙甲 • 苄(有效成分质量比17 : 3)可湿性粉剂相当，持效期达40 d以上。所研制的20%异丙甲 • 苄泡腾片剂表面光滑，无粉尘，使用方便，省时省工，对稻田常见杂草均有良好防效，持效期长，具有推广价值。
- 异丙甲草胺 /
- 苄嘧磺隆 /
- 泡腾片剂 /
- 配方筛选 /
- 稻田杂草 /
- 防治效果
Abstract: In order to improve the labor-saving degree of chemical control of weeds in rice fields and reduce the cost of weed control, metolachlor + bensulfuron-methyl 20% effervescent tablets were prepared by the dry pressing process. The type and dosage of adjuvants in the formulation were selected by the single variable method, and the field efficacy of the prepared effervescent tablets was evaluated. The results showed that the optimal formulation (mass fraction) of metolachlor + bensulfuron-methyl 20% effervescent tablets was: 16% metolachlor, 4% bensulfuron-methyl, 18% organobentonite, 9% white carbon black, 20% tartaric acid, 20% sodium bicarbonate, 6% EFW, 4% G202 and 3% magnesium stearate. The effervescent tablets could effectively control weeds in the rice field in the dosage range of 120-180 g/hm² of active ingredients, and its control efficacy was significantly better than that of single agent, which was equivalent to that of the registered wettable powder. The duration of control efficacy was more than 40 days. The effervescent tablets prepared in the study had smooth surface, no dust, and remarkable control efficacy against weeds in the rice field, which was worth to be promoted as a convenient and time- and labor-saving pesticide formulation.
- metolachlor /
- bensulfuron-methyl /
- effervescent tablets /
- formula screening /
- paddy weed /
- control efficacy

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图 1 泡腾片剂加工工艺流程

Figure 1. Process for the preparation of effervescent tablets

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图 2 不同填料的氮气吸附曲线

Figure 2. Nitrogen adsorption curves of different fillers

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表 1 不同填料的物理性质

Table 1. Physical properties of different fillers

填料名称 Fillers name	颗粒间孔隙率 Interparticle porosity, I_e	流动性 (吸附原油后) Liquidity (After adsorption of crude oil)
填料名称 Fillers name	颗粒间孔隙率 Interparticle porosity, I_e	休止角 Angle of repose, α/(°)	豪斯纳比 Hausner ratio, IH
白炭黑 White carbon black	2.9	16	1.09
高岭土 Kaolin clays	1.0	25	1.31
有机膨润土 Organobentonite	1.1	22	1.22
硅藻土 Kieselguhr	0.4	29	1.36

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表 2 填料选择

Table 2. Filler selection

填料 (m(白炭黑) : m(有机膨润土)=) Fillers (m(silica) : m(organobentonite)=)	崩解时间 Disintegration time/s	悬浮率 Suspensibility/ %	硬度 Hardness/ (kg/mm²)
13.5 : 13.5	410	87.4	4.5
18 : 9	402	86.3	3.2
9: 18	418	89.8	6.9

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表 3 崩解剂选择

Table 3. Disintegrant selection

崩解剂 Disintegrant	质量比 Mass ratio	崩解时间 Disintegration time/s	CO₂释放量 Carbon dioxide release/g	吸湿率 Moisture absorption rate/%
柠檬酸 : 碳酸钠 Citric acid : sodium carbonate	22 : 18	688	0.144	5.1
	21 : 19	650	0.141	5.0
	20 : 20	733	0.132	5.3
	19 : 21	750	0.136	5.1
	18 : 22	834	0.118	4.7
柠檬酸 : 碳酸氢钠 Citric acid : sodium bicarbonate	22 : 18	998	0.082	5.1
	21 : 19	912	0.111	5.0
	20 : 20	860	0.129	5.3
	19 : 21	823	0.150	4.7
	18 : 22	821	0.142	4.9
酒石酸 : 碳酸钠 Tartaric acid : sodium carbonate	22 : 18	680	0.158	5.9
	21 : 19	630	0.182	6.0
	20 : 20	621	0.189	6.3
	19 : 21	650	0.176	6.3
	18 : 22	745	0.134	6.1
酒石酸 : 碳酸氢钠 Tartaric acid : sodium bicarbonate	22 : 18	521	0.161	5.3
	21 : 19	478	0.188	5.8
	20 : 20	407	0.202	5.9
	19 : 21	445	0.192	5.8
	18 : 22	500	0.168	5.6

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表 4 润湿剂选择

Table 4. Wetting agent selection

润湿剂 Wetting agent	质量分数 Mass fraction/%	润湿时间 Wetting time/s
790A	6	69
十二烷基硫酸钠 Sodium lauryl sulfate	6	72
木质素磺酸钠 Sodium lignosulfonate	6	69
烷基萘磺酸盐 (EFW) Alkyl naphthalene sulfonate	6	43

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表 5 分散剂选择

Table 5. Dispersant selection

分散剂 Dispersant	质量分数 Mass fraction/%	悬浮率 Suspensibility/%
十二烷基苯磺酸钠 Sodium dodecyl benzene sulfonate	4	83
亚甲基双萘磺酸钠 NNO	4	81
羧酸盐分散剂 D1003 Carboxylate D1003	4	84
分散剂 202 Greensperse 202 (G202)	4	90

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表 6 润滑剂选择

Table 6. Lubricant selection

润滑剂 Lubricant	质量分数 Mass fraction/%	光滑度 Smoothness	是否黏冲 Whether stick to the punch
滑石粉 Talcum	3	不光滑 Rough	黏冲 Punch sticking
聚乙二醇6000 PEG6000	3	不光滑 Rough	不黏冲 No punch sticking
硬脂酸镁 Magnesium stearate	3	光滑 Smooth	不黏冲 No punch sticking

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表 7 包装材料选择

Table 7. Packaging material selection

包装材料 Packaging materials	稳定性 Stability
水溶袋 Water soluble bag	密闭性差，不崩解 Poor tightness, no disintegration
PE袋 PE bag	密闭性差，不崩解 Poor tightness, no disintegration
铝箔袋 Aluminum foil bag	密闭性强，崩解 Strong tightness, disintegration

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表 8 热贮前后CO₂释放量

Table 8. Release amount of CO₂ before and after the thermal storage

序号 Serial number	单片质量 Tablet mass/g	贮前释放CO₂质量 Mass of carbon dioxide before storage/g	序号 Serial number	单片质量 Tablet weight/g	贮后释放CO₂质量 Mass of carbon dioxide after storage/g
1	0.77	0.193	1	0.79	0.194
2	0.79	0.196	2	0.78	0.196
3	0.81	0.202	3	0.82	0.201
4	0.80	0.198	4	0.81	0.200
5	0.80	0.194	5	0.80	0.193

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表 9 20%异丙甲 • 苄泡腾片热贮稳定性

Table 9. Thermal storage stability of metolachlor + bensulfuron-methyl 20% effervescent tablets

检测项目 Test items	热贮前 Before thermal storage	热贮后 After thermal storage
异丙甲草胺含量 The content of metolachlor/%	16	15.4
苄嘧磺隆含量 The content of bensulfuron-methyl/%	4	3.9
悬浮率 Suspensibility/%	90	88
pH值 pH value	6.9	6.7
崩解时间 Disintegration time/s	418	532
是否胀袋 Whether swollen bag	否 No	否 No

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表 10 20%异丙甲 • 苄泡腾片剂对稻田杂草的株防效和鲜重防效

Table 10. The control efficacy of metolachlor + bensulfuron-methyl 20% effervescent tablets based on the weed number and fresh weight in rice fields

	防治效果 Control efficacy/%
	处理 Treatment	稗草 Echinochloa crusgalli	千金子 Leptochloa chinensis	鳢肠 Eclipta prostrata	莎草 Cyperus rotundus	总草 Total grass
药后 20 d 株防效 Control efficacy of plant number after 20 d	1	93.15 a	83.24 b	95.79 a	91.09 a	91.42 a
	2	96.04 a	89.21 a	97.47 a	92.38 a	94.05 a
	3	34.95 c	25.90 c	86.39 b	89.41 a	60.81 c
	4	87.64 b	82.43 b	83.45 b	83.84 b	84.32 b
	5	94.13 a	82.39 b	95.62 a	91.76 a	91.77 a
药后 40 d 株防效 Control efficacy of plant number after 40 d	1	85.76 a	81.06 a	88.52 a	88.31 a	86.03 a
	2	87.62 a	81.36 a	93.35 a	91.06 a	88.90 a
	3	28.63 c	23.29 b	87.19 a	88.11 a	58.39 c
	4	79.18 b	80.71 a	79.74 b	85.12 b	81.82 b
	5	86.06 a	82.31 a	89.69 a	87.07 ab	86.35 a
药后 40 d 鲜重防效 Control efficacy of fresh weight after 40 d	1	91.77 a	88.62 a	88.86 b	90.03 a	90.05 a
	2	94.97 a	90.78 a	94.57 a	92.37 a	93.19 a
	3	24.51 c	18.31 b	88.84 b	89.27 a	39.95 b
	4	86.93 b	88.49 a	81.06 c	86.95 b	86.45 a
	5	92.26 a	88.65 a	90.26 ab	86.57 b	90.22 a
注：同列数值后含有不同字母表示邓肯新复极差检验法在P < 0.05水平上差异显著。处理1为20%异丙甲 • 苄泡腾片(有效成分120 g/hm²)；处理2为20%异丙甲 • 苄泡腾片(有效成分180 g/hm²)；处理3为10%苄嘧磺隆可湿性粉剂(有效成分120 g/hm²)；处理4为960 g/L异丙甲草胺乳油(有效成分120 g/hm²)；处理5为20%异丙甲 • 苄可湿性粉剂(有效成分120 g/hm²)。Note: Different letters in the same column mean significant differences at P < 0.05 according to a DMRT test. Treatment 1: metolachlor + bensulfuron-methyl 20% effervescent tablets (120 g a.i./hm²). Treatment 2: metolachlor + bensulfuron-methyl 20% effervescent tablets (180 g a.i./hm²). Treatment 3: bensulfuron-methyl 10% WP (120 g a.i./hm²). Treatment 4: metolachlor 960 g/L EC (120 g a.i./hm²). Treatment 5: metolachlor + bensulfuron-methyl 20% WP (120 g a.i./hm²).

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参考文献(26)

[1]	谭卫军, 赵振华, 陈勇. 10%苄嘧磺隆 • 异丙草胺可湿性粉剂对水稻抛秧田杂草的防除作用[J]. 杂草科学, 2015, 33(2): 52-56. TAN W J, ZHAO Z H, CHEN Y. Efficacy of the formulated mixture of bensulfuron methyl-propisochlor on weeds in seedling-broadcasted rice fields[J]. Weed Sci, 2015, 33(2): 52-56.
[2]	中国农药信息网. 农药登记数据[EB/OL]. (2021-09-24). http://www.chinapesticide.org.cn/hysj/index.jhtml. China Pesticide Information Network. Data of pesticideregistration[EB/OL]. (2021-09-24). http://www.chinapesticide.org.cn/hysj/index.jhtml.
[3]	黄坤敏, 高振兴, 史文琦, 等. 20%苄嘧磺隆 • 莎稗磷可湿性粉剂防除水稻移栽田杂草效果[J]. 江西农业学报, 2013, 25(3): 54-57. doi: 10.3969/j.issn.1001-8581.2013.03.016 HUANG K M, GAO Z X, SHI W Q, et al. Control effects of wettable powder of 20% bensulfuron-methyl • anilofos on weeds in transplanted rice field[J]. Acta Agriculturae Jiangxi, 2013, 25(3): 54-57. doi: 10.3969/j.issn.1001-8581.2013.03.016
[4]	刘旺, 袁树忠, 张省委, 等. 国内农药泡腾剂的应用研究概况[J]. 农药, 2019, 58(1): 16-20. LIU W, YUAN S Z, ZHANG S W, et al. Application research of pesticides effervescent formulations[J]. Agrochemicals, 2019, 58(1): 16-20.
[5]	徐会会, 张良菊, 李俊凯, 等. 6%苯醚甲环唑 • 丙环唑泡腾片剂的研制及其毒力测定[J]. 农药, 2017, 56(4): 257-259. XU H H, ZHANG L J, LI J K, et al. The preparation and toxicity test of difenoconazole• propiconazole 6% effervescent tablet[J]. Agrochemicals, 2017, 56(4): 257-259.
[6]	柴金珍, 彭辉, 蒋丽, 等. 国内泡腾片剂型问题与分析[J]. 食品与发酵工业, 2015, 41(9): 243-246. CHAI J Z, PENG H, JIANG L, et al. Domestic effervescent tablets formulation and its problems analysis[J]. Food Ferment Ind, 2015, 41(9): 243-246.
[7]	张宏康, 林奕楠, 李德荣, 等. 番石榴泡腾片固体饮料研制[J]. 食品工业, 2015, 36(1): 4-7. ZHANG H K, LIN Y N, LI D R, et al. Preparation of solid beverage of effervescent tablet from the extract of Psidium guajava[J]. Food Ind, 2015, 36(1): 4-7.
[8]	农药悬浮率测定方法: GB/T 14825—2006[S]. 北京: 中国标准出版社, 2007. Determination method for suspensibility of pesticides: GB/T 14825—2006[S]. Beijing: China Standards Press, 2007.
[9]	农药可湿性粉剂润湿性测定方法: GB/T 5451—2001[S]. 北京: 中国标准出版社, 2001. Testing method for the wettability of dispersible powders of pesticides: GB/T 5451—2001[S]. Beijing: China Standards Press, 2001.
[10]	农药热贮稳定性测定方法: GB/T 19136—2003[S]. 北京: 中国标准出版社, 2003. Testing method for the storage stability at elevated temperature of pesticides: GB/T 19136—2003[S]. Beijing: China Standards Press, 2003.
[11]	刘涛, 付春梅, 唐玉, 等. 基于QbD理念的桑枝泡腾片成型工艺研究[J]. 中药材, 2018, 41(11): 2636-2640. LIU T, FU C M, TANG Y, et al. Research on the forming technology of mulberry effervescent tablets based on QbD concept[J]. J Chin Med Mat, 2018, 41(11): 2636-2640.
[12]	药物引湿性试验指导原则: 中华人民共和国药典2020版四部9103[S]. 北京: 中国医药科技出版社, 2020. Guiding principles for drug hygroscopicity: Pharmacopoeia of the People's Republic of China 2020, Part 4 9103[S]. Beijing: China Medical Science Press, 2020.
[13]	方峰, 赖开平, 叶一强, 等. 15%苄嘧 • 丙草胺泡腾片剂的研制及其药效试验[J]. 化工技术与开发, 2011, 40(10): 1-4. doi: 10.3969/j.issn.1671-9905.2011.11.001 FANG F, LAI K P, YE Y Q, et al. Preparation of 15% bensulfuron-methyl and mefenacet effervescent tablet and its control effect in field[J]. Technol Devel Chem Ind, 2011, 40(10): 1-4. doi: 10.3969/j.issn.1671-9905.2011.11.001
[14]	华乃震. 农药剂型的进展和动向(下)[J]. 农药, 2008, 47(4): 235-239. doi: 10.3969/j.issn.1006-0413.2008.04.001 HUA N Z. Advance and trend of pesticide formulation development[J]. Agrochemicals, 2008, 47(4): 235-239. doi: 10.3969/j.issn.1006-0413.2008.04.001
[15]	董翥飞. 15%苯噻 • 苄泡腾片剂的研制与生物测定[D]. 长春: 吉林农业大学, 2006. DONG Z F. The manufacture of 15% bensulfuron-methyl•mefenacet effervescent tablet and biological tests[D]. Changchun: Jilin Agricultural University, 2006.
[16]	马超, 杜勇, 吴玉辉, 等. 21%丙草胺 • 二氯喹啉酸 • 苄嘧磺隆泡腾片剂的研制[J]. 农药, 2018, 57(10): 716-719. MA C, DU Y, WU Y H, et al. Preparation of pretilachlor • ouinclorac • bensulfuron-methyl 21% effervescent tablet[J]. Agrochemicals, 2018, 57(10): 716-719.
[17]	王学林, 李榆庆, 安燕萍, 等. 28%苄嘧磺隆 • 扑草净泡腾颗粒剂的研制[J]. 农药, 2017, 56(8): 573-576. WANG X L, LI Y Q, AN Y P, et al. Preparation of bensulfuron-methyl • prometryn 28% effervescent granule[J]. Agrochemicals, 2017, 56(8): 573-576.
[18]	赵健鹏, 李树柏, 李波, 等. 1.8%阿维菌素泡腾乳粒剂的研究与制备[J]. 世界农药, 2019, 41(5): 48-52. ZHAO J P, LI S B, LI B, et al. Study and preparation of avermectin 1.8% effervescent emulsion granule[J]. World Pestic, 2019, 41(5): 48-52.
[19]	刘盼西, 李淑兰, 李元广, 等. 海洋芽孢杆菌可湿性粉剂配方的优化[J]. 农药学学报, 2014, 16(2): 206-212. doi: 10.3969/j.issn.1008-7303.2014.02.15 LIU P X, LI S L, LI Y G, et al. Formulation optimization of Bacillus marinus wettable powder[J]. Chin J Pestic Sci, 2014, 16(2): 206-212. doi: 10.3969/j.issn.1008-7303.2014.02.15
[20]	ZHANG S P, WANG J, YANG X D, et al. Impact of EO chain length of dodecanol ethoxylates (C₁₂E_n) on the rheological properties and physical stability of pesticide suspension concentrate[J]. Colloids Surf A Physicochem Eng Aspects, 2021, 627: 127163. doi: 10.1016/j.colsurfa.2021.127163
[21]	华乃震. 农药泡腾剂的加工和应用[J]. 世界农药, 2015, 37(2): 37-42. HUA N Z. Processing and application of pesticides effervescent formulations[J]. World Pestic, 2015, 37(2): 37-42.
[22]	FENG N, ZHANG B, XIN X, et al. Role of aliphatic alcohol polyoxyethylene ether phosphate in 25 wt% tebuconazole suspension concentrate: dispersion and wetting[J]. Colloid Surface A, 2021, 628: 127350. doi: 10.1016/j.colsurfa.2021.127350
[23]	谷祖敏, 邹益泽, 梁玎玎, 等. 鸭跖草致病菌草茎点霉SYAU-06水分散粒剂配方筛选[J]. 农药学学报, 2020, 22(5): 877-883. GU Z M, ZOU Y Z, LIANG D D, et al. Formula selection of Phoma herbarum SYAU-06 water dispersible granule against dayflower[J]. Chin J Pestic Sci, 2020, 22(5): 877-883.
[24]	赖菁华, 杨晓雯. 响应面法优化乌梅泡腾片的配方[J]. 食品工业, 2020, 41(4): 91-95. LAI J H, YANG X W. Optimization on the formula of dark plum effervescent tablets using response surface methodology[J]. Food Ind, 2020, 41(4): 91-95.
[25]	张磊, 王锦旭, 杨贤庆, 等. 合浦珠母贝糖胺聚糖泡腾片制备工艺优化及其质量分析[J]. 大连海洋大学学报, 2018, 33(5): 644-650. ZHANG L, WANG J X, YANG X Q, et al. Optimization of ingredients and quality analysis of effervescent tablets of glycosaminoglycans from pearl oyster Pinctada martensii[J]. J Dalian Ocean Univ, 2018, 33(5): 644-650.
[26]	丁正. 新型Harpin泡腾片剂型的研制及其防治玉米细菌新病害的研究[D]. 南京: 南京农业大学, 2015. DING Z. Studies on Harpin effervescent tablet and using it control an new corn diseases[D]. Nanjing: Nanjing Agricultural University, 2015.