氟吡菌胺和吡唑醚菌酯在葡萄和土壤中的残留分析
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摘要
[目的]建立高效液相色谱法同时检测葡萄、土壤中氟吡菌胺和吡唑醚菌酯残留的方法。[方法]葡萄和土壤样品均用乙腈提取,提取液用PSA及C18吸附剂分散固相萃取净化,高效液相色谱检测,外标法定量。[结果]方法的线性范围为0.05～5.00 mg/L,氟吡菌胺相关系数为1.0000,吡唑醚菌酯相关系数为0.9999;在0.05、0.50、2.00 mg/kg 3个添加水平下,葡萄中氟吡菌胺和吡唑醚菌酯的平均回收率分别为86.7%～97.8%和90.6%～95.6%,相对标准偏差分别为2.55%～8.49%和2.14%～7.80%,土壤中氟吡菌胺和吡唑醚菌酯的平均回收率分别为79.1%～93.6%和83.4%～98.9%,相对标准偏差分别为5.29%～6.78%、1.69%～7.34%;在上述检测条件下,氟吡菌胺的最小检出量(LOD)为0.1 ng,在葡萄和土壤中的最低检测浓度(LOQ)均为0.05 mg/kg;吡唑醚菌酯的最小检出量(LOD)为0.1 ng,在葡萄和土壤中的最低检测浓度(LOQ)均为0.05 mg/kg。[结论]该方法具有简单可靠,分析样品时间短,准确度、精密度和灵敏度符合农药残留分析要求等特点,可以用于同时检测葡萄、土壤上氟吡菌胺和吡唑醚菌酯的残留量。
[Aims] A high performance liquid chromatography(HPLC) method for the simultaneous determination of fluopicolide and pyraclostrobin residues in grapes and soil was established. [Methods] Grape and soil samples were extracted with acetonitrile, and the extracts were purified by solid phase extraction with PSA and C18 adsorbents,detectedbyHPLCandquantified byexternalstandard method. [Results]The linearrange ofthe method was0.05-5.00 mg/L,the correlation coefficient of fluopicolide was 1.0000, the correlation coefficient of pyraclostrobin was 0.9999, and the average recoveries of fluopicolide and pyraclostrobin in grape ranged from 86.7 to 97.8% and 90.6 to 95.6% at the levels of 0.05, 0.50 and 2.00 mg/kg, respectively. The average recoveries of flupiramide and pyraclostrobin in soil ranged from 79.1 to 93.6% and 83.4 to 98.9% respectively with relative standard deviation(RSD) of 1.69-7.34%. The limit of detection(LOD) of fluopicolide was 0.1 ng, and the limit of quantitation(LOQ) in grape and soil was both 0.05 mg/kg.The limit of detection(LOD) of pyraclostrobin was 0.1 ng, and the limit of quantitation(LOQ) of pyraclostrobin in grape and soil was 0.05 mg/kg. [Conclusions] The method is simple, reliable and rapidly. The accuracy, precision and sensitivity meet the requirements of pesticide residue analysis. It can be used for the simultaneous determination of fluopicolide and pyraclostrobin residues in grape and soil.
[Aims] A high performance liquid chromatography(HPLC) method for the simultaneous determination of fluopicolide and pyraclostrobin residues in grapes and soil was established. [Methods] Grape and soil samples were extracted with acetonitrile, and the extracts were purified by solid phase extraction with PSA and C18 adsorbents,detectedbyHPLCandquantified byexternalstandard method. [Results]The linearrange ofthe method was0.05-5.00 mg/L,the correlation coefficient of fluopicolide was 1.0000, the correlation coefficient of pyraclostrobin was 0.9999, and the average recoveries of fluopicolide and pyraclostrobin in grape ranged from 86.7 to 97.8% and 90.6 to 95.6% at the levels of 0.05, 0.50 and 2.00 mg/kg, respectively. The average recoveries of flupiramide and pyraclostrobin in soil ranged from 79.1 to 93.6% and 83.4 to 98.9% respectively with relative standard deviation(RSD) of 1.69-7.34%. The limit of detection(LOD) of fluopicolide was 0.1 ng, and the limit of quantitation(LOQ) in grape and soil was both 0.05 mg/kg.The limit of detection(LOD) of pyraclostrobin was 0.1 ng, and the limit of quantitation(LOQ) of pyraclostrobin in grape and soil was 0.05 mg/kg. [Conclusions] The method is simple, reliable and rapidly. The accuracy, precision and sensitivity meet the requirements of pesticide residue analysis. It can be used for the simultaneous determination of fluopicolide and pyraclostrobin residues in grape and soil.
引文
[1] PALMIERI M C, PERAZZOLLI M, MATAFORA V, et al.Proteomic Analysis of Grapevine Resistance Induced by Trichodermaharzianum T39 Reveals Specific Defence Pathways Activatedagainst Downy Mildew[J]. J Exp Bot, 2012(63):6237-6251.
[2]唐兴敏,孙磊,张玮,等.葡萄霜霉病抗病性鉴定方法及品种抗病性测定[J].植物保护, 2018, 44(1):166-169.
[3]刘新秀,张莉,任毓忠,等.葡萄品种抗霜霉病不同鉴定方法的比较和相关性分析[J].新疆农业科学, 2012, 49(7):1244-1249.
[4]司伟杰,张涛,梅向东,等.含氟农药的研究进展[J].河北工业科技, 2014, 31(3):262-270.
[5]关爱莹,李慧超,张金波,等.甲氧基丙烯酸酯类杀菌剂的发展沿革及几个主要品种的合成[J].精细与专用化学品, 2012, 20(4):24-28.
[6]郭延蕊,梁晨,李宝笃,等.氟吡菌胺对大白菜霜霉病的作用方式和持效期[J].农药, 2014, 53(5):372-374.
[7]石磊,张洁,邸云红,等. 68.75%氟吡菌胺-霜霉威悬浮液对马铃薯晚疫病的防效[J].农技服务, 2017, 34(18):60-63.
[8]张小军,张宗俭,刘尚钟,等.氟吡菌胺原药的高效液相色谱分析[J].农药, 2011, 50(9):661-662.
[9]傅强,聂思桥,任竞,等.戊唑醇和吡唑醚菌酯在玉米植株和土壤中残留及其消解动态的检测[J].湖南农业大学学报(自然科学版), 2015, 41(6):661-665.
[10]石凯威,郑尊涛,马成,等.吡唑醚菌酯在苹果和土壤中的消解及安全性评价[J].农药, 2015, 54(1):45-48.
[11] FU Jian-tao, LI Zi-hao, HUANG Ri-lin, et al. Dissipation,Residue, and Distribution of Pyraclostrobin in Banana and Soilunder Field Conditions in South China[J]. International Journalof Environmental Analytical Chemistry, 2016, 96:1367-1377.
[12] GUO Xin-yan, WU Wen-zhu, SONG Ning-hui, et al. ResidueDynamics and Risk Assessment of Pyraclostrobin in Rice,Plants, Hulls, Field Soil, and Paddy Water, Human and EcologicalRisk Assessment[J]. An International Journal, 2016, 23:67-81.
[2]唐兴敏,孙磊,张玮,等.葡萄霜霉病抗病性鉴定方法及品种抗病性测定[J].植物保护, 2018, 44(1):166-169.
[3]刘新秀,张莉,任毓忠,等.葡萄品种抗霜霉病不同鉴定方法的比较和相关性分析[J].新疆农业科学, 2012, 49(7):1244-1249.
[4]司伟杰,张涛,梅向东,等.含氟农药的研究进展[J].河北工业科技, 2014, 31(3):262-270.
[5]关爱莹,李慧超,张金波,等.甲氧基丙烯酸酯类杀菌剂的发展沿革及几个主要品种的合成[J].精细与专用化学品, 2012, 20(4):24-28.
[6]郭延蕊,梁晨,李宝笃,等.氟吡菌胺对大白菜霜霉病的作用方式和持效期[J].农药, 2014, 53(5):372-374.
[7]石磊,张洁,邸云红,等. 68.75%氟吡菌胺-霜霉威悬浮液对马铃薯晚疫病的防效[J].农技服务, 2017, 34(18):60-63.
[8]张小军,张宗俭,刘尚钟,等.氟吡菌胺原药的高效液相色谱分析[J].农药, 2011, 50(9):661-662.
[9]傅强,聂思桥,任竞,等.戊唑醇和吡唑醚菌酯在玉米植株和土壤中残留及其消解动态的检测[J].湖南农业大学学报(自然科学版), 2015, 41(6):661-665.
[10]石凯威,郑尊涛,马成,等.吡唑醚菌酯在苹果和土壤中的消解及安全性评价[J].农药, 2015, 54(1):45-48.
[11] FU Jian-tao, LI Zi-hao, HUANG Ri-lin, et al. Dissipation,Residue, and Distribution of Pyraclostrobin in Banana and Soilunder Field Conditions in South China[J]. International Journalof Environmental Analytical Chemistry, 2016, 96:1367-1377.
[12] GUO Xin-yan, WU Wen-zhu, SONG Ning-hui, et al. ResidueDynamics and Risk Assessment of Pyraclostrobin in Rice,Plants, Hulls, Field Soil, and Paddy Water, Human and EcologicalRisk Assessment[J]. An International Journal, 2016, 23:67-81.