毒死蜱、吡虫啉、螺虫乙酯及其代谢物和苯醚甲环唑在梨中的残留消解动态
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摘要
利用仪器分析方法和田间试验法,研究了毒死蜱、吡虫啉、螺虫乙酯及其代谢物和苯醚甲环唑在梨中的残留消解动态。样品经乙腈提取,氯化钠盐析净化,毒死蜱采用气相色谱-质谱联用仪检测,其他3种农药采用液相色谱-质谱联用仪检测,外标法定量。结果表明:毒死蜱、吡虫啉、螺虫乙酯及其代谢物和苯醚甲环唑4种农药在梨中的消解动态均满足一级反应动力学方程,半衰期分别为4.4、12.2、13.1和10.3 d。施药后7 d至收获期,4种农药在梨中的最终残留量均未超出中国国家标准中规定的最大残留限量值,按照推荐剂量及其操作规范在梨上施用是安全的。
The instrument anlysis method and field testing method were employed for the investigation3 of the dissipation dynamics and residues of chlorpyrifos, imidacloprid,spirotetramat and its motablites,difenoconazole, in pear. The samples were extracted with acetonitrile and purified by sodium chloride salting out. Chlorpyrifos was detected by GC/MS/MS, and the other three pesticides were detected by LC/MS/MS. Quantization was performed using external standard method. The results showed that the dissipation dynamics of chlorpyrifos, imidacloprid, spirotetramat and its motablites, difenoconazole, in pear meet the first-degree dynamics matrix. There half-lives were 4.4, 12.2, 13.1 and 10.3 d,respectively. From 7 days after the pesticide application to harvest, the final residues of the above 4 pesticides in pear did not exceed the MRL value of China. According to the recommended application concentration and operating procedures, All four pesticides can be safely used on pears.
The instrument anlysis method and field testing method were employed for the investigation3 of the dissipation dynamics and residues of chlorpyrifos, imidacloprid,spirotetramat and its motablites,difenoconazole, in pear. The samples were extracted with acetonitrile and purified by sodium chloride salting out. Chlorpyrifos was detected by GC/MS/MS, and the other three pesticides were detected by LC/MS/MS. Quantization was performed using external standard method. The results showed that the dissipation dynamics of chlorpyrifos, imidacloprid, spirotetramat and its motablites, difenoconazole, in pear meet the first-degree dynamics matrix. There half-lives were 4.4, 12.2, 13.1 and 10.3 d,respectively. From 7 days after the pesticide application to harvest, the final residues of the above 4 pesticides in pear did not exceed the MRL value of China. According to the recommended application concentration and operating procedures, All four pesticides can be safely used on pears.
引文
[1]现代农业产业技术体系管理平台.国家梨产业技术体系[EB/OL].(2018-05-20). http://123.127.160.231/index.do?method=center&product=%C0%E6&productId=029China Agriculture Research System. National pear research system[EB/OL].(2018-05-20). http://123.127.160.231/index.do?method=center&product=%C0%E6&productd=029
[2]聂继云,李志霞,刘传德,等.苹果农药残留风险评估[J].中国农业科学, 2014, 47(18):3655-3667.NIE J Y, LI Z X, LIU C D, et al. Risk assessment of pesticide residues in apples[J]. Scientia Agricultura Sinica, 2014, 47(18):3655-3667.
[3]刘纲华,龚道新,黄雪.苯醚甲环唑在黄瓜及土壤中的残留消解行为研究[J].作物研究, 2013, 27(1):40-45.LIU G H, GONG D X, HUANG X. Residue and degradation behavior of difenoconazole in cucumber and its soil[J]. Crop Res, 2013, 27(1):40-45.
[4]仇微,王亚南,魏铁松,等.苯醚甲环唑在套袋与不套袋苹果中的残留及消解动态[J].农药学学报, 2013, 15(4):451-456.QIU W, WANG Y N, WEI T S, et al. Residue and dissipation dynamics of difenoconazole in bagged and non-bagged apples[J].Chin J Pestic Sci, 2013, 15(4):451-456.
[5]黄玉南,张绍铃,方金豹,等.吡虫啉在梨果实中的残留动态分析[J].果树学报, 2010, 27(3):453-456.HUANG Y N, ZHANG S L, FANG J B, et al. Study on residue trends of imidacloprid in pear fruit[J]. J Fruit Sci, 2010, 27(3):453-456.
[6]吴迪,王跃进,张伟国,等.离子交换固相萃取-高效液相色谱法研究吡虫啉在梨中的分布及残留动态[J].分析测试学报, 2007, 26(5):682-685.WU D, WANG Y J, ZHANG W G, et al. Determination of imidacloprid residue and its distribution in pears by SCX-solid-phase extraction-high performance liquid chromatography[J]. J Instrum Anal, 2007, 26(5):682-685.
[7]赵丽娟,张洪,秦曙,等.毒死蜱在梨和土壤中的残留研究[J].农药科学与管理, 2010, 31(2):42-46.ZHAO L J, ZHANG H, QIN S, et al. Study on the chlorpyrifos residues in pear and soil[J]. Pestic Sci Admin, 2010, 31(2):42-46.
[8]张莹,师校欣,杜国强,等.毒死蜱在梨果实不同部位的残留及消解动态[J].农药学学报, 2017, 19(2):231-237.ZHANG Y, SHI X X, DU G Q, et al. Residue and dissipation of chlorpyrifos in different tissues of Pyrus bretschneideri Rehd[J]. Chin J Pestic Sci, 2017, 19(2):231-237.
[9]李刚波,樊继德,赵林,等.五种套袋对早熟梨果实糖酸和毒死蜱农药残留的影响[J].浙江农业学报, 2018, 30(8):1363-1368.LI G B, FAN J D, ZHAO L, et al. Effects of 5 bagging treatments on sugar and acid content and chlorpyrifos pesticide residues in early maturing pears[J]. Acta Agriculturae Zhejiangensis, 2018, 30(8):1363-1368.
[10]吴育佳,杨仁斌,聂红英.螺虫乙酯在黄瓜及其土壤中残留量检测方法及残留规律研究[J].中国农学通报, 2015, 31(35):110-115.WU Y J, YANG R B, NIE H Y. Study on residual detection method and residue rule of spirotetramat in cucumber and soil[J]. Chin Agric Sci Bull, 2015, 31(35):110-115.
[11]孟志远,任莉,宋玥颐,等.液相色谱-串联质谱法同时测定菠菜、土壤及水体中螺虫乙酯及4种代谢物残留[J].农药学学报, 2017,19(4):482-490.MENG Z Y, REN L, SONG Y Y, et al. Simultaneous determination of spirotetramat and its four metabolites in Spinacia oleracea L., soil and water using liquid chromatography tandem mass spectrometry[J].Chin J Pestic Sci, 2017, 19(4):482-490.
[12]农药残留试验准则:NY/T 788–2004[S].北京:中国农业出版社,2004.Guideline on pesticide residue trials:NY/T 788–2004[S]. Beijing:China Agriculture Press, 2004.
[13]王运浩.农药登记残留田间试验标准操作规程[M].北京:中国标准出版社, 2007.WANG Y H. Standard operating procedures on pesticide registration residue field trials[M]. Beijing:Standards Press of China, 2007.
[14]食品安全国家标准食品中农药最大残留限量2017[M].北京:中国标准出版社, 2017.National food safety standard-Maximum residue limits for pesticide in food. 2017[M]. Beijing:Standards Press of China, 2017.
[15]中国农药信息网.农药登记信息[EB/OL].[2017-11-20].http://www.chinapesticide.gov.cn/.China Pesticide Information Network. Information of pesticide registration[EB/OL].[2017-11-20]. http://www.chinapesticide.gov.cn/.
[2]聂继云,李志霞,刘传德,等.苹果农药残留风险评估[J].中国农业科学, 2014, 47(18):3655-3667.NIE J Y, LI Z X, LIU C D, et al. Risk assessment of pesticide residues in apples[J]. Scientia Agricultura Sinica, 2014, 47(18):3655-3667.
[3]刘纲华,龚道新,黄雪.苯醚甲环唑在黄瓜及土壤中的残留消解行为研究[J].作物研究, 2013, 27(1):40-45.LIU G H, GONG D X, HUANG X. Residue and degradation behavior of difenoconazole in cucumber and its soil[J]. Crop Res, 2013, 27(1):40-45.
[4]仇微,王亚南,魏铁松,等.苯醚甲环唑在套袋与不套袋苹果中的残留及消解动态[J].农药学学报, 2013, 15(4):451-456.QIU W, WANG Y N, WEI T S, et al. Residue and dissipation dynamics of difenoconazole in bagged and non-bagged apples[J].Chin J Pestic Sci, 2013, 15(4):451-456.
[5]黄玉南,张绍铃,方金豹,等.吡虫啉在梨果实中的残留动态分析[J].果树学报, 2010, 27(3):453-456.HUANG Y N, ZHANG S L, FANG J B, et al. Study on residue trends of imidacloprid in pear fruit[J]. J Fruit Sci, 2010, 27(3):453-456.
[6]吴迪,王跃进,张伟国,等.离子交换固相萃取-高效液相色谱法研究吡虫啉在梨中的分布及残留动态[J].分析测试学报, 2007, 26(5):682-685.WU D, WANG Y J, ZHANG W G, et al. Determination of imidacloprid residue and its distribution in pears by SCX-solid-phase extraction-high performance liquid chromatography[J]. J Instrum Anal, 2007, 26(5):682-685.
[7]赵丽娟,张洪,秦曙,等.毒死蜱在梨和土壤中的残留研究[J].农药科学与管理, 2010, 31(2):42-46.ZHAO L J, ZHANG H, QIN S, et al. Study on the chlorpyrifos residues in pear and soil[J]. Pestic Sci Admin, 2010, 31(2):42-46.
[8]张莹,师校欣,杜国强,等.毒死蜱在梨果实不同部位的残留及消解动态[J].农药学学报, 2017, 19(2):231-237.ZHANG Y, SHI X X, DU G Q, et al. Residue and dissipation of chlorpyrifos in different tissues of Pyrus bretschneideri Rehd[J]. Chin J Pestic Sci, 2017, 19(2):231-237.
[9]李刚波,樊继德,赵林,等.五种套袋对早熟梨果实糖酸和毒死蜱农药残留的影响[J].浙江农业学报, 2018, 30(8):1363-1368.LI G B, FAN J D, ZHAO L, et al. Effects of 5 bagging treatments on sugar and acid content and chlorpyrifos pesticide residues in early maturing pears[J]. Acta Agriculturae Zhejiangensis, 2018, 30(8):1363-1368.
[10]吴育佳,杨仁斌,聂红英.螺虫乙酯在黄瓜及其土壤中残留量检测方法及残留规律研究[J].中国农学通报, 2015, 31(35):110-115.WU Y J, YANG R B, NIE H Y. Study on residual detection method and residue rule of spirotetramat in cucumber and soil[J]. Chin Agric Sci Bull, 2015, 31(35):110-115.
[11]孟志远,任莉,宋玥颐,等.液相色谱-串联质谱法同时测定菠菜、土壤及水体中螺虫乙酯及4种代谢物残留[J].农药学学报, 2017,19(4):482-490.MENG Z Y, REN L, SONG Y Y, et al. Simultaneous determination of spirotetramat and its four metabolites in Spinacia oleracea L., soil and water using liquid chromatography tandem mass spectrometry[J].Chin J Pestic Sci, 2017, 19(4):482-490.
[12]农药残留试验准则:NY/T 788–2004[S].北京:中国农业出版社,2004.Guideline on pesticide residue trials:NY/T 788–2004[S]. Beijing:China Agriculture Press, 2004.
[13]王运浩.农药登记残留田间试验标准操作规程[M].北京:中国标准出版社, 2007.WANG Y H. Standard operating procedures on pesticide registration residue field trials[M]. Beijing:Standards Press of China, 2007.
[14]食品安全国家标准食品中农药最大残留限量2017[M].北京:中国标准出版社, 2017.National food safety standard-Maximum residue limits for pesticide in food. 2017[M]. Beijing:Standards Press of China, 2017.
[15]中国农药信息网.农药登记信息[EB/OL].[2017-11-20].http://www.chinapesticide.gov.cn/.China Pesticide Information Network. Information of pesticide registration[EB/OL].[2017-11-20]. http://www.chinapesticide.gov.cn/.