高效液相色谱-串联质谱法测定氰氟虫腙和甲氧虫酰肼在水稻和土壤中的残留及消解动态
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摘要
[目的]建立同时对水稻和土壤中氰氟虫腙和甲氧虫酰肼残留进行测定的高效液相色谱-串联质谱分析方法,研究其在水稻和土壤中的残留及消解动态。[方法]样品中的氰氟虫腙和甲氧虫酰肼经乙腈提取,十八烷基硅烷键合相(C_(18))净化,高效液相色谱-串联质谱(HPLC-MS/MS)检测。[结果]氰氟虫腙和甲氧虫酰肼在水稻植株中的半衰期分别为2.4～11.4、1.3～10.2 d;在土壤中的半衰期分别为3.0～6.8、0.8～10.4 d;在水稻植株中的最终残留量分别为0.213～1.072、0.300～4.757 mg/L,在稻壳中的最终残留量分别为0.040～0.636、0.174～2.257 mg/L,在糙米中的最终残留量均<0.030 mg/L,在土壤中的最终残留量均<1.150 mg/L。[结论]对结果进行分析,建议我国20%氰氟虫腙·甲氧虫酰肼悬浮剂施药剂量的高剂量按制剂量750 g/hm~2 (150 g a.i./hm~2),施药次数为1次。
[Aims] A method was developed for analysis of metaflumizone and methoxyfenozide residues in rice and soil by high performance liquid chromatography-mass spectrum, the residue degradation trend was researched.[Methods] Metaflumizone and methoxyfenozide in rice and soil were extracted with acetonitrile and purified by Octadecylsilane bonded phase, detected by HPLC-MS/MS. [Results] The dissipation half-lives of metaflumizone and methoxyfenozide in rice plant were 2.4-11.4 and 1.3-10.2 d, the half-lives in soil were 3.0-6.8 and 0.8-10.4, respectively. The final residues of metaflumizone and methoxyfenozide in rice plant were 0.213-1.072 and 0.300-4.757 mg/L, the final residues in rice husk were 0.040-0.636 and 0.174-2.257 mg/L, the final residues in brown rice were <0.030 mg/L, the final residues in soil were <1.150 mg/L. [Conclusions] According to the research results, it is suggested that the recommended dosage of metaflumizone·methoxyfenozide 20% SC is 750 g/ha(150 g a.i./ha), application frequency is the one time and the safety interval is 7 d.
[Aims] A method was developed for analysis of metaflumizone and methoxyfenozide residues in rice and soil by high performance liquid chromatography-mass spectrum, the residue degradation trend was researched.[Methods] Metaflumizone and methoxyfenozide in rice and soil were extracted with acetonitrile and purified by Octadecylsilane bonded phase, detected by HPLC-MS/MS. [Results] The dissipation half-lives of metaflumizone and methoxyfenozide in rice plant were 2.4-11.4 and 1.3-10.2 d, the half-lives in soil were 3.0-6.8 and 0.8-10.4, respectively. The final residues of metaflumizone and methoxyfenozide in rice plant were 0.213-1.072 and 0.300-4.757 mg/L, the final residues in rice husk were 0.040-0.636 and 0.174-2.257 mg/L, the final residues in brown rice were <0.030 mg/L, the final residues in soil were <1.150 mg/L. [Conclusions] According to the research results, it is suggested that the recommended dosage of metaflumizone·methoxyfenozide 20% SC is 750 g/ha(150 g a.i./ha), application frequency is the one time and the safety interval is 7 d.
引文
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[6]李燕芳,肖汉祥,李怡峰,等.40%氰氟虫腙·甲氧虫酰肼悬浮剂防治稻纵卷叶螟田间试验[J].现代农业科技,2017(8):94-96.
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[8]SMAGGHE G,PINEDA S,CARTON B,et al.The Chemical and Biological Properties of Methoxyfenozide,A New Insecticidal Ecdysteroid Agonist[J].Pest Management Science,2015,57(2):115-119.
[9]朱丽梅.一个新的蜕皮激素拮抗剂---甲氧虫酰肼[J].世界农药,2001,23(6):50-52.
[10]毛江胜,赵善仓,邓立刚.高效液相色谱法测定菠菜中残留的甲氧虫酰肼[J].农药,2006,45(2):121-122.
[11]章虎,吴俐勤,谢磊,等.高效液相色谱法测定甘蓝、青菜和番茄中虫酰肼、甲氧虫酰肼和呋喃虫酰肼残留[J].现代科学仪器,2006(3):55-58.
[12]KEVIN T,DAVID E,SUSAN M N,et al.Finding of Pesticides in Fashionable Fruit Juices by LC-MS/MS and GC-MS/MS[J].Food Chemistry,2012,134(4):2398-2405.
[13]彭茂民,刘丽,王小飞,等.UPLC-MS-MS法快速测定大白菜和土壤中氰氟虫腙残留[J].湖北农业科学,2016,55(23):6231-6234.
[14]赵成林,刘菲菲,朱国念,等.超高效液相色谱-串联质谱法分析水稻及稻田土壤中残留的氰氟虫腙[J].农药,2013,52(5):357-359.
[15]占绣萍,陈建波,马琳,等.超高效液相色谱-质谱联用法快速测定蔬菜中氰氟虫腙残留[J].农药,2014,53(7):497-511.
[16]郭庆龙,崔淑华,刘靖靖,等.高效液相色谱-串联质谱法测定果蔬中6种新型杀虫剂残留[J].化学通报,2013,76(10):951-956.
[17]戴琳,徐锦忠,丁涛,等.高效液相色谱-电喷雾串联质谱法测定蔬菜中虫酰肼和甲氧虫酰肼残留[J].分析化学,2008(1):87-90.
[2]MCLEESE D W,ZITKO V,SERGEANT D B.Lethality and Accumulation of Alkylphenols in Aquatic Fauma[J].Chemosphere,1981,10(7):723-730.
[3]孙星星,张俊喜,周加春,等.氰氟虫腙的作用机制及抗药性研究进展[J].江苏农业科学,2016,44(3):150-153.
[4]SALGADO V L,HAYASHI J H.Methaflumizone is a Novelsodium Channel Blocker Insecticide[J].Veterinary Parasitology,2007,150:182-189.
[5]GLENN R CARLSON,TARLOCHAN S DHADIALLA,RICKYHUNTER,et al.The Chemical and Biological Properties of Methoxyfeno-zide,A New Insecticidal Ecdysteroid Agonist[J].Pest Management Science,2001,57:115-245.
[6]李燕芳,肖汉祥,李怡峰,等.40%氰氟虫腙·甲氧虫酰肼悬浮剂防治稻纵卷叶螟田间试验[J].现代农业科技,2017(8):94-96.
[7]王胜得,柳爱平,杨春明.酰肼类昆虫生长调节剂的研究进展[J].广东化工,2004(5):37-41.
[8]SMAGGHE G,PINEDA S,CARTON B,et al.The Chemical and Biological Properties of Methoxyfenozide,A New Insecticidal Ecdysteroid Agonist[J].Pest Management Science,2015,57(2):115-119.
[9]朱丽梅.一个新的蜕皮激素拮抗剂---甲氧虫酰肼[J].世界农药,2001,23(6):50-52.
[10]毛江胜,赵善仓,邓立刚.高效液相色谱法测定菠菜中残留的甲氧虫酰肼[J].农药,2006,45(2):121-122.
[11]章虎,吴俐勤,谢磊,等.高效液相色谱法测定甘蓝、青菜和番茄中虫酰肼、甲氧虫酰肼和呋喃虫酰肼残留[J].现代科学仪器,2006(3):55-58.
[12]KEVIN T,DAVID E,SUSAN M N,et al.Finding of Pesticides in Fashionable Fruit Juices by LC-MS/MS and GC-MS/MS[J].Food Chemistry,2012,134(4):2398-2405.
[13]彭茂民,刘丽,王小飞,等.UPLC-MS-MS法快速测定大白菜和土壤中氰氟虫腙残留[J].湖北农业科学,2016,55(23):6231-6234.
[14]赵成林,刘菲菲,朱国念,等.超高效液相色谱-串联质谱法分析水稻及稻田土壤中残留的氰氟虫腙[J].农药,2013,52(5):357-359.
[15]占绣萍,陈建波,马琳,等.超高效液相色谱-质谱联用法快速测定蔬菜中氰氟虫腙残留[J].农药,2014,53(7):497-511.
[16]郭庆龙,崔淑华,刘靖靖,等.高效液相色谱-串联质谱法测定果蔬中6种新型杀虫剂残留[J].化学通报,2013,76(10):951-956.
[17]戴琳,徐锦忠,丁涛,等.高效液相色谱-电喷雾串联质谱法测定蔬菜中虫酰肼和甲氧虫酰肼残留[J].分析化学,2008(1):87-90.