高级搜索

超高效液相色谱串联质谱法测定霜霉威在番茄和土壤中残留及消解动态

,  ,  ,  ,  ,  ,  , 

downloadPDF

上一篇

下一篇

柳亚男, 李敏敏, 范蓓, 卢嘉, 贺妍, 孔志强, 孙玉凤, 王凤忠. 超高效液相色谱串联质谱法测定霜霉威在番茄和土壤中残留及消解动态[J]. 环境化学, 2015, 34(6): 1072-1077. doi: 10.7524/j.issn.0254-6108.2015.06.2014120404
引用本文: 柳亚男, 李敏敏, 范蓓, 卢嘉, 贺妍, 孔志强, 孙玉凤, 王凤忠. 超高效液相色谱串联质谱法测定霜霉威在番茄和土壤中残留及消解动态[J]. 环境化学, 2015, 34(6): 1072-1077. doi: 10.7524/j.issn.0254-6108.2015.06.2014120404
shu
LIU Yanan, LI Minmin, FAN Bei, LU Jia, HE Yan, KONG Zhiqiang, SUN Yufeng, WANG Fengzhong. Residues and dissipation of propamocarb in tomatoes and soil using UPLC-MS/MS[J]. Environmental Chemistry, 2015, 34(6): 1072-1077. doi: 10.7524/j.issn.0254-6108.2015.06.2014120404
Citation: LIU Yanan, LI Minmin, FAN Bei, LU Jia, HE Yan, KONG Zhiqiang, SUN Yufeng, WANG Fengzhong. Residues and dissipation of propamocarb in tomatoes and soil using UPLC-MS/MS[J]. Environmental Chemistry, 2015, 34(6): 1072-1077. doi: 10.7524/j.issn.0254-6108.2015.06.2014120404
shu

超高效液相色谱串联质谱法测定霜霉威在番茄和土壤中残留及消解动态

  • 1.

    中国农业科学院农产品加工研究所农业部农产品加工质量安全风险评估实验室(北京)/农业部农产品加工综合性重点实验室, 北京, 100193

  • 基金项目:

    国家自然科学基金(31401580, 31301477)资助.

Residues and dissipation of propamocarb in tomatoes and soil using UPLC-MS/MS

  • 1.

    Institute of Agro-products Processing Science and Technology, Chinese Academy of Agricultural Sciences, Laboratory of Agro-products Quality Safety Risk Assessment, Ministry of Agriculture, Key Laboratory of Agro-products Processing, Ministry of Agriculture, Beijing, 100193, China

  • Fund Project:

  • 摘要: 应用所建立的分散固相萃取-液相色谱-串联质谱法测定土壤和番茄中霜霉威为0.02、0.20、2.00 mg·kg-1等3个添加浓度时,日内平均回收率为83.9%—104.6%,日内相对标准偏差为1.0%—5.5%,日间平均回收率为84.3%—108.9%,日间相对标准偏差为1.4%—4.9%.霜霉威在1.0—200.0 μg·L-1浓度范围内相关系数R2>0.9992,在土壤中和番茄基质中定量限均为0.02 mg·kg-1.该方法能够满足现有限量标准的要求.霜霉威消解动态试验采用推荐高剂量(90 g·ha-1)为施药剂量,在植株第2穗果膨大期开始喷药1次,分别测定喷药后2 h、1 d、2 d、4 d、7 d、14 d的霜霉威残留量的变化.浙江杭州、山东潍坊和河南商丘的3个试验点消解动态试验中,降解动态符合一级动力学指数模型.2011—2012年霜霉威在番茄中降解半衰期为2.4—4.7 d,在土壤中降解半衰期1.1—1.5 d.施药5 d后的残留量均小于检测限,远远低于2.0 mg·kg-1最大残留限量,实际样品中霜霉威的残留量均低于检测限.72.2%霜霉威水剂按照推荐剂量1.5倍喷施番茄1次,其喷施2 h后的残留量仅为1.5 mg·kg-1,符合残留要求可以安全使用.
    Abstract: The dissipation of propamocarb in tomato and soil was studied to formulate a scientific basis for the acceptable dose and the pre-harvest interval. Dissipation experiments were conducted by applying propamocarb once on tomato and soil with hole application at 90 g·ha-1 after fruit enlargement. The samples were collected randomly from each plot at different time intervals i.e, 2 h, 1, 2, 4, 7, 14 days after the application. Dispersive solid phase extraction combined to ultra-high performance liquid chromatography-tandemmass spectrometry (UPLC-MS/MS) method was used to determine the propamocarb residue in tomato and soil. Recovery test was processed in three spiked levels of 0.02, 0.20 and 2.00 mg·kg-1. The results showed that the within-day average recovery rate of propamocarb in tomato and soil were 83.9%—104.6%, the within-day RSDs were 1.0%—5.5%; the between-day average recovery rate were 84.3%—108.9%, the between-day RSDs were 1.4%—4.9%. The correlation coefficient of propamocarb in the range of 1.0—200.0 μg·L-1 was R2>0.9992, LOQ were 0.02 mg·kg-1. The actual samples and field experimental samples were detected by using this method, the results showed that the degradation half-life of propamocarb in tomato and soil were 2.4—4.7 d and 1.1—1.5 d, respectively. The residues were less than max residue limits (MRLs). The propamocarb agent (72.2%) applied with hole application can be considered safe after more than 2 h in the application to the pre-harvest intervals.
  • 加载中
  • [1]
    [2] 冯大军.霜霉威—霜霉病防治首选药[J]. 果农之友, 2011, (3):32-33
    [3] 吴鹏.黄瓜低霜霉威残留性的生理生化及分子基础研究[D]. 哈尔滨:东北农业大学博士学位论文, 2013
    [4] Wu P. Propamocarb effects on antioxidant parameters and osmolyte levels of cucumber fruit differing in propamocarb residual capacity[J]. Research Journal of Biotechnology, 2014, 9(6): 99-104
    [5] Sahoo S K, Mandal K, Kumar R, et al. Analysis of fluopicolide and propamocarb residues on tomato and soil using QuEChERS sample preparation method in combination with GLC and GCMS[J]. Food Analytical Methods, 2014, 7(5): 1032-1042
    [6] Samoucha Y, Cohen Y. Toxicity of propamocarb to the late blight fungus on potato[J]. Phytoparasitica, 1990, 18(1): 27-40
    [7] Moorman G W, Kim S H. Species of pythium from greenhouses in pennsylvania exhibit resistance to propamocarb and mefenoxam[J]. Plant Disease, 2004, 88(6): 630-632
    [8] Schmuck G, Mihail F. Effects of the carbamates fenoxycarb, propamocarb and propoxur on energy supply, glucose utilization and SH-groups in neurons[J]. Archives of toxicology, 2004, 78(6): 330-337
    [9] Diwan K, Patel A R, Vaghela K M, et al. Dissipation of fluopicolide and propamocarb hydrochloride as combination product in/on tomato (Lycopersicon esculentum) [J]. Pesticide Research Journal, 2013, 25(1): 55-59
    [10] Xiang Y, Zhu W. Determination of propamocarb technical by GC with internal standard analysis method[J]. Agrochemicals, 2013, 7:10-11
    [11] 马佰慧, 秦志伟, 谭行之, 等.利用气相色谱检测黄瓜果实中霜霉威的残留量[J].长江蔬菜, 2010, (20):51-53
    [12] 李飞飞, 黄荣茂, 胡德禹, 等.气相色谱测定土壤中霜霉威的残留[J].农药, 2010, 49(2):131-132
    [13] Abd-Alrahman S H, Almaz M M. Degradation of propamocarb-hydrochloride in tomatoes, potatoes and cucumber using HPLC-DAD and QuEChERS methodology[J]. Bulletin of Environmental Contamination and Toxicology, 2012, 89(2): 302-305.
    [14] 刘润珠, 张靖坤, 崔淑华, 等.气相色谱-质谱法测定大葱基质中霜霉威残留量[J]. 分析测试学报, 2012, 31(z1):34-36
    [15] 李敏敏, 刘新刚, 董丰收, 等. 80%胺鲜酯·甲哌鎓在棉花和土壤中的残留及消解动态[J]. 环境化学, 2013, 32(2): 289-294
    [16] Hiemstra M, de Kok A. Determination of propamocarb in vegetables using polymer-based high-performance liquid chromatography coupled with electrospray mass spectrometry[J]. Journal of Chromatography A, 2002, 972(2): 231-239
    [17] Sahoo S K, Battu R S, Singh B. Development and validation of QuEChERS method for estimation of propamocarb residues in tomato (Lycopersicon esculentum Mill) and soil[J]. American Journal of Analytical Chemistry, 2011, 2(8): 26-31.
    [18] 杜鹏强, 顾晓军, 刘新刚, 等. 气相色谱-电子捕获检测器同时测定食用菌及其拌料中百菌清和高效氯氰菊酯[J]. 环境化学, 2014, 33(3): 459-463
    [19] Anastassiades M, Lehotay S J, Štajnbaher D, et al. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and "dispersive solid-phase extraction" for the determination of pesticide residues in produce[J]. Journal of AOAC International, 2003, 86(2): 412-431
    [20] 张学杰, 付萌, 郭科, 等.霜霉威吡虫啉腐霉利在结球生菜上的消解动态及相关因子的影响[J]. 农业环境科学学报, 2010, 29(1):180-184
    [21] Wang C, Wang Y, Gao J, et al. Dissipation and residues determination of propamocarb in ginseng and soil by high-performance liquid chromatography coupled with tandem mass spectrometry[J]. Environmental Monitoring and Assessment, 2014: 1-10
    [22] Sahoo S K, Battu R S, Singh B. Development and validation of QuEChERS method for estimation of propamocarb residues in tomato (Lycopersicon esculentum Mill) and soil[J]. American Journal of Analytical Chemistry, 2011, 2: 26
    [23] Al-Rahman S H A, Almaz M M, Ahmed N S. Dissipation of fungicides, insecticides, and acaricide in tomato using HPLC-DAD and QuEChERS methodology[J]. Food Analytical Methods, 2012, 5(3): 564-570
  • 加载中
WeChat 点击查看大图
计量
  • 文章访问数:  1768
  • HTML全文浏览数:  1688
  • PDF下载数:  468
  • 施引文献:  0
出版历程
  • 收稿日期:  2014-12-04
  • 刊出日期:  2015-06-15
柳亚男, 李敏敏, 范蓓, 卢嘉, 贺妍, 孔志强, 孙玉凤, 王凤忠. 超高效液相色谱串联质谱法测定霜霉威在番茄和土壤中残留及消解动态[J]. 环境化学, 2015, 34(6): 1072-1077. doi: 10.7524/j.issn.0254-6108.2015.06.2014120404
引用本文: 柳亚男, 李敏敏, 范蓓, 卢嘉, 贺妍, 孔志强, 孙玉凤, 王凤忠. 超高效液相色谱串联质谱法测定霜霉威在番茄和土壤中残留及消解动态[J]. 环境化学, 2015, 34(6): 1072-1077. doi: 10.7524/j.issn.0254-6108.2015.06.2014120404
shu
LIU Yanan, LI Minmin, FAN Bei, LU Jia, HE Yan, KONG Zhiqiang, SUN Yufeng, WANG Fengzhong. Residues and dissipation of propamocarb in tomatoes and soil using UPLC-MS/MS[J]. Environmental Chemistry, 2015, 34(6): 1072-1077. doi: 10.7524/j.issn.0254-6108.2015.06.2014120404
Citation: LIU Yanan, LI Minmin, FAN Bei, LU Jia, HE Yan, KONG Zhiqiang, SUN Yufeng, WANG Fengzhong. Residues and dissipation of propamocarb in tomatoes and soil using UPLC-MS/MS[J]. Environmental Chemistry, 2015, 34(6): 1072-1077. doi: 10.7524/j.issn.0254-6108.2015.06.2014120404
shu

超高效液相色谱串联质谱法测定霜霉威在番茄和土壤中残留及消解动态

  • 1. 中国农业科学院农产品加工研究所农业部农产品加工质量安全风险评估实验室(北京)/农业部农产品加工综合性重点实验室, 北京, 100193
  • 收稿日期:  2014-12-04
基金项目:

国家自然科学基金(31401580, 31301477)资助.

摘要: 应用所建立的分散固相萃取-液相色谱-串联质谱法测定土壤和番茄中霜霉威为0.02、0.20、2.00 mg·kg-1等3个添加浓度时,日内平均回收率为83.9%—104.6%,日内相对标准偏差为1.0%—5.5%,日间平均回收率为84.3%—108.9%,日间相对标准偏差为1.4%—4.9%.霜霉威在1.0—200.0 μg·L-1浓度范围内相关系数R2>0.9992,在土壤中和番茄基质中定量限均为0.02 mg·kg-1.该方法能够满足现有限量标准的要求.霜霉威消解动态试验采用推荐高剂量(90 g·ha-1)为施药剂量,在植株第2穗果膨大期开始喷药1次,分别测定喷药后2 h、1 d、2 d、4 d、7 d、14 d的霜霉威残留量的变化.浙江杭州、山东潍坊和河南商丘的3个试验点消解动态试验中,降解动态符合一级动力学指数模型.2011—2012年霜霉威在番茄中降解半衰期为2.4—4.7 d,在土壤中降解半衰期1.1—1.5 d.施药5 d后的残留量均小于检测限,远远低于2.0 mg·kg-1最大残留限量,实际样品中霜霉威的残留量均低于检测限.72.2%霜霉威水剂按照推荐剂量1.5倍喷施番茄1次,其喷施2 h后的残留量仅为1.5 mg·kg-1,符合残留要求可以安全使用.

English Abstract

    全文HTML

参考文献 (23)

返回顶部

目录

/

返回文章
返回

Copyright © 2019 中国科学院生态环境研究中心