气相色谱-串联质谱法同时测定蔬菜中4种杀菌剂残留量
Simultaneous GC-MS/MS Determination of Residual Amounts of 4 Fungicides in Vegetables
摘 要
提出了气相色谱-串联质谱法同时测定蔬菜中甲霜灵、腐霉利、苯醚甲环唑和恶唑菌酮等4种杀菌剂残留量的方法。蔬菜样品经乙酸乙酯提取浓缩后,乙酸乙酯溶解。用BR-5MS毛细管色谱柱为固定相进行色谱分离,质谱分析中采用多反应监测模式。4种杀菌剂的质量浓度均在0.05~0.40 mg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.001~0.029 mg·L-1之间。以空白样品为基体进行加标回收试验,所得回收率在75.6%~102%之间,测定值的相对标准偏差(n=6)在0.6%~6.2%之间。
杀菌剂
蔬菜
GC-MS/MS
Fungicides
Vegetable
Abstract
A method of GC-MS/MS for the simultaneous determination of residual amounts of 4 fungicides,i.e. metalaxyl,procymidone,difenoconazole and famoxadone in vegetables was proposed. The vegetable sample was extracted with ethyl acetate and concentrated,the residue was taken up with ethyl acetate. The BR-5MS capillary chromatographic column was used for GC separation and the multiple reaction monitoring mode was adopted in MS determination. Linear relationships between values of peak area and mass concentration of the 4 fungicides were kept in the same range of 0.05-0.40 mg·L-1,with detection limits (3S/N) in the range of 0.001-0.029 mg·L-1. On the base of blank sample,test for recovery was made by standard addition method; values of recovery found were in the range of 75.6%-102%,with RSD′s (n=6) in the range of 0.6%-6.2%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201511019
所属栏目 工作简报
基金项目
收稿日期 2014/11/21
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网络出版日期
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备注陈君义(1983-),男,河南西峡人,工程师,硕士,主 要从事进出口产品理化分析。
引用该论文: CHEN Jun-yi,SUN Hui-yu,WANG Yun-fei. Simultaneous GC-MS/MS Determination of Residual Amounts of 4 Fungicides in Vegetables[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(11): 1572～1575
陈君义,孙慧宇,王云飞. 气相色谱-串联质谱法同时测定蔬菜中4种杀菌剂残留量[J]. 理化检验－化学分册, 2015, 51(11): 1572～1575
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参考文献
【1】李锋格,全晓盾,窦辉,等.气相色谱-质谱法测定番茄酱中甲霜灵、苯霜灵和恶霜灵的残留量［J］.中国卫生检验杂志,2007,17(3):388-389.
【2】卢晓宇,陈跃,王金华,等.气相色谱-质谱联用法测定食品中腐霉利残留量［J］.北京化工大学学报,2008,35(3):35-38.
【3】沈伟健,杨雯筌,沈崇钰,等.气相色谱-负化学离子源法检测食品中苯醚甲环唑的残留量［J］.色谱,2007,25(3):418-421.
【4】李彦文,郭正元,杨仁斌,等.柑橘中恶唑菌酮残留量的气相色谱分析［J］.色谱,2005,23(3):327-327.
【5】李彦文,杨仁斌.恶唑菌酮的环境行为及残留毒理研究现状［J］.环境保护科学,2006,32(5):47-49.
【6】徐国锋,聂继云,李静,等.苹果、香蕉和柑橘中腐霉利等4种防腐保鲜剂残留分析方法［J］.农药学学报,2009,11(3):351-356.
【7】郑龙,周敏.气相色谱-质谱联用法测定蔬菜中的腐霉利残留试验［J］.广东农业科学,2009,36(3):155-156.
【8】王连珠,王登飞,郑俊超,等.气相色谱-质谱法测定荷兰豆中氟硅唑、丙环唑、苯醚甲环唑残留量［J］.理化检验-化学分册,2006,42(12):1025-1028.
【9】黎其万,刘宏程,张玉荣,等.雪莲果中甲霜灵、异菌脲和除虫脲残留量的高效液相色谱测定方法［J］.分析试验室,2007,26(12):83-86.
【10】任刚,廖卫波,胡志成,等.人参提取物中腐霉利残留的HPLC分析［J］.中国实验方剂学杂志,2013,19(23):107-110.
【11】徐浩,李振,赵华,等.恶唑菌酮在柑橘上的残留动态研究［J］.浙江农业学报,2006,18(4):273-276.
【12】王远,邢丽杰,郝家勇,等.高效液相色谱-串联质谱法测定蔬菜中苯醚甲环唑的残留量［J］.食品科学,2011,32(18):296-299.
【13】李彦文,杨仁斌,郭正元,等.恶唑菌酮在柑橘土壤中的残留动态研究［J］.环境科学与技术,2006,29(6):11-13.
【14】OLIVA J,NAVARRO S,BARBA A,et al. Determination of chlorpyrifos,penconazole,fenarimol,vinclozolin and metalaxyl in grapes,must and wine by on-line microextraction and gas chromatography［J］. Journal of Chromatography A,1999,833(1):43-51.
【15】张雪燕,吴文锐,毛佳,等.气相色谱法测定三七中苯醚甲环唑残留［J］.湖南农业大学学报,2010,36(2):229-232.
【16】FENOLL J,HELLN P,MARTNEZ C M,et al. Pesticide residue analysis of vegetables by gas chromatography with electron-capture detection［J］. Journal of AOAC International,2007,90(1):263-270.
【17】代雪芳,毛佳,张雪燕,等.苯醚甲环唑在香蕉和土壤中的残留分析方法研究［J］.分析试验室,2010,29(5):66-68.
【18】SN/T 2230-2008 进出口食品中腐霉利残留量的检测方法 气相色谱-质谱法［S］.
【19】CHEN Li,LI Xue-sheng,WANG Zheng-quan,et al. Residue dynamics of procymidone in leeks and soils in greenhouses by smoke generator application［J］. Ecotoxicology and Environmental Safety,2010,73(1):73-77.
【20】钱宗耀,周晓龙,刘河疆,等.气质联用法测定红枣中苯醚甲环唑残留量［J］.现代农药,2012,11(3):37-39.
【2】卢晓宇,陈跃,王金华,等.气相色谱-质谱联用法测定食品中腐霉利残留量［J］.北京化工大学学报,2008,35(3):35-38.
【3】沈伟健,杨雯筌,沈崇钰,等.气相色谱-负化学离子源法检测食品中苯醚甲环唑的残留量［J］.色谱,2007,25(3):418-421.
【4】李彦文,郭正元,杨仁斌,等.柑橘中恶唑菌酮残留量的气相色谱分析［J］.色谱,2005,23(3):327-327.
【5】李彦文,杨仁斌.恶唑菌酮的环境行为及残留毒理研究现状［J］.环境保护科学,2006,32(5):47-49.
【6】徐国锋,聂继云,李静,等.苹果、香蕉和柑橘中腐霉利等4种防腐保鲜剂残留分析方法［J］.农药学学报,2009,11(3):351-356.
【7】郑龙,周敏.气相色谱-质谱联用法测定蔬菜中的腐霉利残留试验［J］.广东农业科学,2009,36(3):155-156.
【8】王连珠,王登飞,郑俊超,等.气相色谱-质谱法测定荷兰豆中氟硅唑、丙环唑、苯醚甲环唑残留量［J］.理化检验-化学分册,2006,42(12):1025-1028.
【9】黎其万,刘宏程,张玉荣,等.雪莲果中甲霜灵、异菌脲和除虫脲残留量的高效液相色谱测定方法［J］.分析试验室,2007,26(12):83-86.
【10】任刚,廖卫波,胡志成,等.人参提取物中腐霉利残留的HPLC分析［J］.中国实验方剂学杂志,2013,19(23):107-110.
【11】徐浩,李振,赵华,等.恶唑菌酮在柑橘上的残留动态研究［J］.浙江农业学报,2006,18(4):273-276.
【12】王远,邢丽杰,郝家勇,等.高效液相色谱-串联质谱法测定蔬菜中苯醚甲环唑的残留量［J］.食品科学,2011,32(18):296-299.
【13】李彦文,杨仁斌,郭正元,等.恶唑菌酮在柑橘土壤中的残留动态研究［J］.环境科学与技术,2006,29(6):11-13.
【14】OLIVA J,NAVARRO S,BARBA A,et al. Determination of chlorpyrifos,penconazole,fenarimol,vinclozolin and metalaxyl in grapes,must and wine by on-line microextraction and gas chromatography［J］. Journal of Chromatography A,1999,833(1):43-51.
【15】张雪燕,吴文锐,毛佳,等.气相色谱法测定三七中苯醚甲环唑残留［J］.湖南农业大学学报,2010,36(2):229-232.
【16】FENOLL J,HELLN P,MARTNEZ C M,et al. Pesticide residue analysis of vegetables by gas chromatography with electron-capture detection［J］. Journal of AOAC International,2007,90(1):263-270.
【17】代雪芳,毛佳,张雪燕,等.苯醚甲环唑在香蕉和土壤中的残留分析方法研究［J］.分析试验室,2010,29(5):66-68.
【18】SN/T 2230-2008 进出口食品中腐霉利残留量的检测方法 气相色谱-质谱法［S］.
【19】CHEN Li,LI Xue-sheng,WANG Zheng-quan,et al. Residue dynamics of procymidone in leeks and soils in greenhouses by smoke generator application［J］. Ecotoxicology and Environmental Safety,2010,73(1):73-77.
【20】钱宗耀,周晓龙,刘河疆,等.气质联用法测定红枣中苯醚甲环唑残留量［J］.现代农药,2012,11(3):37-39.
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