氟虫腈在水稻上的残留动态及降解菌的筛选
摘要
本文改进了稻米、小麦、玉米等谷物及水稻秸秆和土壤中氟虫腈残留量检测方法,研究了80%氟虫腈水分散粒剂在水稻和土壤中的残留消解动态及最终残留量;同时从农药厂污泥中分离出一株可降解氟虫腈的细菌。主要研究结果如下:
1.样品中氟虫腈残留采用乙腈为提取溶剂、超声波振荡提取,谷物及秸秆提取液经柱层析净化,采用气相色谱电子俘获检测器检测。在0.01~0.5mg/kg的添加浓度范围内,氟虫腈的平均回收率在80.60%~99.66%之间,相对标准偏差低于9%,最小检测浓度为0.01mg/kg。方法的灵敏度与精密度符合农药残留分析要求。
2. 80%氟虫腈水分散粒剂在水稻植株中的消解符合一级动力学模型,安徽合肥地区水稻植株中氟虫腈消解较慢,半衰期约为10.0d,在湖南长沙地区的消解则较快,半衰期约为4.6d。80%氟虫腈水分散粒剂按2倍推荐最高剂量(相当于72g a.i/hm2)喷洒施药,在土壤中残留量经过由低到高,再由高到低的过程,其中在第7天残留量达到最高,45d后土壤中氟虫腈的残留量在0.2mg/kg左右。
3. 80%氟虫腈水分散粒剂按36g(ai)/hm2和72g(ai)/hm2分别喷施1次和2次(喷洒间隔7d),距最后一次施药21d后,氟虫腈在两地土壤、水稻植株、稻米和稻壳中最终残留量分别为1.14~6.85mg/kg、0.03~0.32mg/kg、0.01~0.11mg/kg和0.07~1.42mg/kg。
4.从农药厂污泥中筛选出一株对氟虫腈降解能力较强和生长较快的菌株。氟虫腈浓度为50mg/L时,培养5天的降解率达到81%,半衰期最短为2.4d,降解速率为0.3548d-1,相对于空白对照中氟虫腈消解速率的1.90倍。
5.筛选得到的菌株在30℃、pH 7.0和1%(W/V)的NaCl条件下生长,镜检呈现直杆状,两端钝圆,菌落不透明,略有粉红色,革兰氏染色为阴性。初步鉴定为沙雷氏菌属。
In this study, a method was developed to analysis residue of fipronil in cereal and soil.The degradation and final residues of fipronil in rice and soil were studied through field experiments in Anhui and Hunan with different dosages and spraying methods.Μsing enrichment medium and inorganic salt medium, a fipronil degrading strain was isolated from sludge and identified as actinomyces. The main results of this paper were shown as follows:
1. A method was developed to analysis residue of fipronil in cereal and soil. After acetonitrile was added, the samples were sonicated in anμltrasonic water bath and then centrifuged, filtered, and cleaned up by a column containing neutral alumina and active carbon, successive eluted by ethyl acetate /n-hexane (3:5,V/V). The pesticide residues were determined by gas chromatography with electron-capture detection. Recoveries at spiked concentrations between 0.01 to 0.5mg/kg were 80.60%~99.66% with RSDs less than 9%. The limit of detection was 0.01mg/kg. The sensitivity and accuracy of the proposed method were fit for analysis of pesticide residue in cereal and soil.
2. The degradation of fipronil in plant was fit for first-order kinetic model, that in Hefei was slower (the half-lives were 10 days) than in Hunan (the half-lives were 4.6 days).After spraying fipronil 80% WG at recommended double dosage (equivalent to 72 g a.i/hm2), the residue in soil was increasing until 7th day, and then decreased. The final residue in soil was about 0.2mg/kg after 45 days.
3. Fipronil 80% WG was sprayed into the rice field once and twice at 36 g a.i/hm2 and 72 g a.i/hm2. The maximum residue levels of fipronil in soil, straw, rice and bran were 1.14~6.85mg/kg, 0.03~0.32mg/kg, 0.01~0.11mg/kg and 0.07~1.42mg/kg twenty-one days later.
4. A strain which can degrade fipronil and grow rapidly was isolated and selected from the soil of pesticide factory. The degradation rate for 50mg/L fipronil can reach 81% in 5 days. Compared to the unspiked one, the rate enhanced 1.9 times.
5. The strain lived at the condition of 30℃,PH 7.0 and NaCl of 1%(W/V).It is straight rod-shaped which is round at both sides.The colony is opaque with the color of pink.It showed negative by gram stain. It was preliminarily identified as S.Marcescens.
1.样品中氟虫腈残留采用乙腈为提取溶剂、超声波振荡提取,谷物及秸秆提取液经柱层析净化,采用气相色谱电子俘获检测器检测。在0.01~0.5mg/kg的添加浓度范围内,氟虫腈的平均回收率在80.60%~99.66%之间,相对标准偏差低于9%,最小检测浓度为0.01mg/kg。方法的灵敏度与精密度符合农药残留分析要求。
2. 80%氟虫腈水分散粒剂在水稻植株中的消解符合一级动力学模型,安徽合肥地区水稻植株中氟虫腈消解较慢,半衰期约为10.0d,在湖南长沙地区的消解则较快,半衰期约为4.6d。80%氟虫腈水分散粒剂按2倍推荐最高剂量(相当于72g a.i/hm2)喷洒施药,在土壤中残留量经过由低到高,再由高到低的过程,其中在第7天残留量达到最高,45d后土壤中氟虫腈的残留量在0.2mg/kg左右。
3. 80%氟虫腈水分散粒剂按36g(ai)/hm2和72g(ai)/hm2分别喷施1次和2次(喷洒间隔7d),距最后一次施药21d后,氟虫腈在两地土壤、水稻植株、稻米和稻壳中最终残留量分别为1.14~6.85mg/kg、0.03~0.32mg/kg、0.01~0.11mg/kg和0.07~1.42mg/kg。
4.从农药厂污泥中筛选出一株对氟虫腈降解能力较强和生长较快的菌株。氟虫腈浓度为50mg/L时,培养5天的降解率达到81%,半衰期最短为2.4d,降解速率为0.3548d-1,相对于空白对照中氟虫腈消解速率的1.90倍。
5.筛选得到的菌株在30℃、pH 7.0和1%(W/V)的NaCl条件下生长,镜检呈现直杆状,两端钝圆,菌落不透明,略有粉红色,革兰氏染色为阴性。初步鉴定为沙雷氏菌属。
In this study, a method was developed to analysis residue of fipronil in cereal and soil.The degradation and final residues of fipronil in rice and soil were studied through field experiments in Anhui and Hunan with different dosages and spraying methods.Μsing enrichment medium and inorganic salt medium, a fipronil degrading strain was isolated from sludge and identified as actinomyces. The main results of this paper were shown as follows:
1. A method was developed to analysis residue of fipronil in cereal and soil. After acetonitrile was added, the samples were sonicated in anμltrasonic water bath and then centrifuged, filtered, and cleaned up by a column containing neutral alumina and active carbon, successive eluted by ethyl acetate /n-hexane (3:5,V/V). The pesticide residues were determined by gas chromatography with electron-capture detection. Recoveries at spiked concentrations between 0.01 to 0.5mg/kg were 80.60%~99.66% with RSDs less than 9%. The limit of detection was 0.01mg/kg. The sensitivity and accuracy of the proposed method were fit for analysis of pesticide residue in cereal and soil.
2. The degradation of fipronil in plant was fit for first-order kinetic model, that in Hefei was slower (the half-lives were 10 days) than in Hunan (the half-lives were 4.6 days).After spraying fipronil 80% WG at recommended double dosage (equivalent to 72 g a.i/hm2), the residue in soil was increasing until 7th day, and then decreased. The final residue in soil was about 0.2mg/kg after 45 days.
3. Fipronil 80% WG was sprayed into the rice field once and twice at 36 g a.i/hm2 and 72 g a.i/hm2. The maximum residue levels of fipronil in soil, straw, rice and bran were 1.14~6.85mg/kg, 0.03~0.32mg/kg, 0.01~0.11mg/kg and 0.07~1.42mg/kg twenty-one days later.
4. A strain which can degrade fipronil and grow rapidly was isolated and selected from the soil of pesticide factory. The degradation rate for 50mg/L fipronil can reach 81% in 5 days. Compared to the unspiked one, the rate enhanced 1.9 times.
5. The strain lived at the condition of 30℃,PH 7.0 and NaCl of 1%(W/V).It is straight rod-shaped which is round at both sides.The colony is opaque with the color of pink.It showed negative by gram stain. It was preliminarily identified as S.Marcescens.
引文
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[2]成四喜,吴放军.新型吡唑类广谱杀虫剂氟虫腈的合成和应用.农药译丛, 1995:17(1):18~21
[3]牛洪涛,罗万春,江改清等.氟虫腈对小菜蛾生物活性及田间防治效果.植物保护学报, 2007:34(3):45~46
[4]郭慧芳,束兆林等.氟虫腈对水稻害虫的作用特点及应用.植物保护学报, 2001,28(3):12~17
[5]朱金文,魏方林,李少南等.氟虫腈对家蚕的急性毒性与安全评价研究.农药学学报, 2006,8(1):141~145
[6]邓荣臻,周婷.氟虫腈对蜜蜂风险调查的反思.蜜蜂杂志.2008,28(10):22~23
[7]农业部办公厅.第八届全国农药登记评审委员会第四次全体会议纪要.2009:1~16
[8]Bobe A,Coste D.M,J.Cooper. Factors influencing the adsorption of fipronil on soils. In:Agriculture Food Chemistry,1997,45:4861-4865
[9]BurrC M. Adsorption to and from four soils and one sediment. ,1997, No.520:62-241
[10]Μ.S. Environmental Protection Agency. New Pesticide Fact Sheet. Pesticide and toxic substances. May 1996
[11]朱国念,吴金涛,刘乾开等.氟虫腈在模拟稻田生态系统中降解途径的研究.农药学学报,2000,6(2):52～56
[12]周培,陆贻通,吴银良.锐劲特在水稻上的残留动态研究.农业环境保护,2001,20(5):360~362
[13]陆贻通,周培,吴银良.锐劲特在菜地生态系统中的残留动态研究.环境污染与防治,2001,23(5):219~221
[14]何艺兵.氟虫腈在甘蓝和土壤中的残留分析方法.农业科学与管理, 2000,21(3):17~19
[15]吴风燕,张红艳,刘丰茂等.氟虫腈在甘蓝及土壤中的残留动态研究.农业环境科学学报,2006,25(增刊):265~268
[16]操海群,施艳红,花日茂等.氟虫腈在番茄和土壤中残留分析方法的研究.安徽农业大学学报,2005,32(1):31~35
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