绿豆和向日葵中福美双的残留分析
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摘要
[目的]建立气相色谱-电子捕获检测器(GC-ECD)检测绿豆和向日葵中福美双残留量的方法,为18%辛硫磷·福美双微囊悬浮剂在绿豆和向日葵上的田间应用提供科学用药参考。[方法]实验研究根据GB 2763—2014规定,将福美双衍生化为CS_2。样品在SnCl_2·HCl溶液中加热到85℃分解产生CS_2,正己烷吸收CS_2,GC-ECD检测,仪器的最小检出量(LOD)为2.52×10~(-11)g,最低检测质量分数(LOQ)为0.08 mg/kg。[结果]绿豆和向日葵中的福美双添加质量分数为0.13、0.67、5.33 mg/kg时,福美双在绿豆中的平均回收率为86.24%~101.72%,相对标准偏差为0.99%~5.10%,在向日葵中平均回收率为83.64%~100.52%,相对标准偏差为1.00%~5.60%。田间试验研究结果显示,福美双在绿豆和向日葵中的最终残留量(福美双转化为CS_2,以CS_2计)均低于0.08 mg/kg。[结论]绿豆按18%辛硫磷·福美双微囊悬浮剂推荐剂量1∶(80~53)(药种比)的制剂用量施用,向日葵按推荐剂量1∶(17~25)(药种比)的制剂用量施用,收获的成熟绿豆和向日葵是安全的。
[Aims] A gas chromatography-electron capture detector(GC-ECD) method for determination of thiram residues in mung bean and sunflower was developed to provide a reference for the rational use of phoxim·thiram 18%microcapsule suspension in the field. [Methods] According to the national standard GB 2763—2014, thiram was derivatized to carbon disulfide, then carbon disulfide was extracted with n-hexane and determined by gas chromatography-electron capture detector. The limits of detection(LOD) were 2.52 ×10~(-11) g, and the limits of quantitation(LOQ) were 0.08 mg/kg. [Results] When the spiked levels were 0.13, 0.67 and 5.33 mg/kg, the recoveries of thiram in mung bean were 86.24-101.72% with the relative standard deviations of 0.99-5.10%; the recoveries of thiram in sunflower were 83.64-100.52% with the relative standard deviations of 1.00-5.60%. The final residues of thiram in mung bean and sunflower were less than 0.08 mg/kg(measured as CS_2). [Conclusions] Mung bean and sunflower were treated with phoxim·thiram 18% microcapsule suspension at the recommended dose of 1∶(80-53) and1∶(17-25)(mass ratio), respectively. The final residues of thiram in mung bean and sunflower were safely at harvest.
[Aims] A gas chromatography-electron capture detector(GC-ECD) method for determination of thiram residues in mung bean and sunflower was developed to provide a reference for the rational use of phoxim·thiram 18%microcapsule suspension in the field. [Methods] According to the national standard GB 2763—2014, thiram was derivatized to carbon disulfide, then carbon disulfide was extracted with n-hexane and determined by gas chromatography-electron capture detector. The limits of detection(LOD) were 2.52 ×10~(-11) g, and the limits of quantitation(LOQ) were 0.08 mg/kg. [Results] When the spiked levels were 0.13, 0.67 and 5.33 mg/kg, the recoveries of thiram in mung bean were 86.24-101.72% with the relative standard deviations of 0.99-5.10%; the recoveries of thiram in sunflower were 83.64-100.52% with the relative standard deviations of 1.00-5.60%. The final residues of thiram in mung bean and sunflower were less than 0.08 mg/kg(measured as CS_2). [Conclusions] Mung bean and sunflower were treated with phoxim·thiram 18% microcapsule suspension at the recommended dose of 1∶(80-53) and1∶(17-25)(mass ratio), respectively. The final residues of thiram in mung bean and sunflower were safely at harvest.
引文
[1]VERMA B C,SOOD R K,SIDHU H S.A New Colorimetric Method for the Determination of Carbon Disulphide and Its Application to the Analysis of Some Dithiocarbamate Fungicides[J].Talanta,1983,30(10):787-788.
[2]陈上进.50%福美双可湿性粉剂防治水稻稻瘟病的田间试验[J].广西植保,2008,21(4):11-12.
[3]师勇强,冯自力,李志芳,等.400 g·L-1福美双·萎锈灵悬浮种衣剂对棉花苗期立枯病的防治效果[J].中国棉花,2014,41(9):28-30.
[4]束兆林,杨红福,缪康,等.咪鲜胺与福美双及其混剂对小麦赤霉病菌的抑制效果与增效研究[J].农学学报,2015,5(4):40-43.
[5]陈景莲,徐利敏,于传宗.6%福美双·戊唑醇·氯氰菊酯悬浮种衣剂防治玉米丝黑穗病药效试验[J].内蒙古农业科技,2012,11(1):69-70.
[6]陈多永.80%福美双·福美锌WP防治西瓜炭疽病田间药效试验[J].安徽农学通报,2009,15(3):178,202.
[7]陈申宽,闫路海,刘玉良,等.35.6%阿维菌素、多菌灵、福美双悬浮种衣剂对大豆苗期病虫害的防治试验[J].植物医生,2008,21(3):38-40.
[8]胡健,仇广灿,成晓松.80%多菌灵·福美双WP防治番茄叶霉病田间药效试验简报[J].上海农业科技,2009,12(2):107.
[9]何献声,孙利.40%啶菌恶唑·福美双悬浮剂防治黄瓜灰霉病田间药效试验初探[J].农药,2012,51(4):310-311.
[10]BEBE F N,PANEMANGALORE M.Pestcides in the Diet Modify the Retention of Calcium,Zinc and Copper Metals in the Small Intenstines[J].FASEB J,2004,18(4):364.
[11]DALVI P S,WILDER-OFIE T,MARES B.Effect of Cytochrome P450 Inducers on the Metabolisim and Toxicity of Thiram in Rats[J].Vet Hum Toxicol,2002,44(6):331-333.
[12]孟凡立,崔兆丰,王志坤,等.高效液相色谱法检测福美双在蔬菜及土壤中的残留[J].东北农业大学学报,2010,41(6):28-31.
[13]宋国春,于建垒,李美,等.福美双在棉花及土壤中残留量分析方法[J].农药科学与管理,2000,21(5):13-23.
[14]李恒,杨仁斌,蒋为,等.福美双在水稻和稻田土壤中残留动态研究[J].农药科学与管理,2009,30(2):26-29.
[15]覃慧丽,谭辉华,李雪生,等.高效液相色谱法测定香蕉和土壤中福美双的残留量[J].农药,2013,52(10):740-742.
[16]李伟华,胡小宁,吕雪霞,等.比色法快速测定小麦中福美双的残留量[J].农药,2011,50(3):213-214.
[17]黄永忠,魏东,杨彩玲.15%福美双·吡虫啉·烯唑醇悬浮种衣剂的RP-HPLC分析[J].农药,2008,47(2):114-115.
[18]董广新,周良佳,杜薇.40%啶菌恶唑·福美双悬乳剂高效液相色谱分析[J].农药,2005,44(12):551-552.
[19]俞幼芬.吡虫啉、拌种灵和福美双三元复配种衣剂分析方法研究[J].农药,2001,40(4):22.
[20]刘淑凤,孙式吉,戎鹏举,吕静珍.紫外分光光度法测定福美双含量[J].农药,1985(1):34-35.
[21]王颖,郭兴杰.福美双的分光光度测定法[J].农药,1994,33(5):20.
[22]诸本贤.福美双的比色测定[J].农药,1983,21(5):17-39.
[2]陈上进.50%福美双可湿性粉剂防治水稻稻瘟病的田间试验[J].广西植保,2008,21(4):11-12.
[3]师勇强,冯自力,李志芳,等.400 g·L-1福美双·萎锈灵悬浮种衣剂对棉花苗期立枯病的防治效果[J].中国棉花,2014,41(9):28-30.
[4]束兆林,杨红福,缪康,等.咪鲜胺与福美双及其混剂对小麦赤霉病菌的抑制效果与增效研究[J].农学学报,2015,5(4):40-43.
[5]陈景莲,徐利敏,于传宗.6%福美双·戊唑醇·氯氰菊酯悬浮种衣剂防治玉米丝黑穗病药效试验[J].内蒙古农业科技,2012,11(1):69-70.
[6]陈多永.80%福美双·福美锌WP防治西瓜炭疽病田间药效试验[J].安徽农学通报,2009,15(3):178,202.
[7]陈申宽,闫路海,刘玉良,等.35.6%阿维菌素、多菌灵、福美双悬浮种衣剂对大豆苗期病虫害的防治试验[J].植物医生,2008,21(3):38-40.
[8]胡健,仇广灿,成晓松.80%多菌灵·福美双WP防治番茄叶霉病田间药效试验简报[J].上海农业科技,2009,12(2):107.
[9]何献声,孙利.40%啶菌恶唑·福美双悬浮剂防治黄瓜灰霉病田间药效试验初探[J].农药,2012,51(4):310-311.
[10]BEBE F N,PANEMANGALORE M.Pestcides in the Diet Modify the Retention of Calcium,Zinc and Copper Metals in the Small Intenstines[J].FASEB J,2004,18(4):364.
[11]DALVI P S,WILDER-OFIE T,MARES B.Effect of Cytochrome P450 Inducers on the Metabolisim and Toxicity of Thiram in Rats[J].Vet Hum Toxicol,2002,44(6):331-333.
[12]孟凡立,崔兆丰,王志坤,等.高效液相色谱法检测福美双在蔬菜及土壤中的残留[J].东北农业大学学报,2010,41(6):28-31.
[13]宋国春,于建垒,李美,等.福美双在棉花及土壤中残留量分析方法[J].农药科学与管理,2000,21(5):13-23.
[14]李恒,杨仁斌,蒋为,等.福美双在水稻和稻田土壤中残留动态研究[J].农药科学与管理,2009,30(2):26-29.
[15]覃慧丽,谭辉华,李雪生,等.高效液相色谱法测定香蕉和土壤中福美双的残留量[J].农药,2013,52(10):740-742.
[16]李伟华,胡小宁,吕雪霞,等.比色法快速测定小麦中福美双的残留量[J].农药,2011,50(3):213-214.
[17]黄永忠,魏东,杨彩玲.15%福美双·吡虫啉·烯唑醇悬浮种衣剂的RP-HPLC分析[J].农药,2008,47(2):114-115.
[18]董广新,周良佳,杜薇.40%啶菌恶唑·福美双悬乳剂高效液相色谱分析[J].农药,2005,44(12):551-552.
[19]俞幼芬.吡虫啉、拌种灵和福美双三元复配种衣剂分析方法研究[J].农药,2001,40(4):22.
[20]刘淑凤,孙式吉,戎鹏举,吕静珍.紫外分光光度法测定福美双含量[J].农药,1985(1):34-35.
[21]王颖,郭兴杰.福美双的分光光度测定法[J].农药,1994,33(5):20.
[22]诸本贤.福美双的比色测定[J].农药,1983,21(5):17-39.