GC-MS Determination of Residual Amount of Spirotetramat in Vegetables and Fruits
摘 要
采用气相色谱-质谱法测定蔬菜和水果中螺虫乙酯的残留量。蔬菜或水果样品经乙腈均质提取,以乙二胺-N-丙基硅烷和十八烷基硅烷为基质分散固相萃取剂净化。在气相色谱分离中用HP-5MS毛细管色谱柱为固定相,在质谱分析中采用选择离子监测模式。螺虫乙酯的质量浓度在10~500 μg·L-1内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.75 μg·kg-1,测定下限(10S/N)为2.51 μg·kg-1。以空白样品为基体进行加标回收试验,所得回收率为79.8%~101%,测定值的相对标准偏差(n=6)为4.1%~8.7%。
Abstract
GC-MS was applied to the determination of residual amount of spirotetramat in vegetables and fruits. The sample of vegetable or fruit was extracted with acetonitrile homogeneously, and purified by matrix dispersion solid phase extraction with PSA and C18. The HP-5MS capillary chromatographic column was used for GC separation and the selected ion monitoring mode was adopted in MS determination. Linear relationship between values of peak area and mass concentration of spirotetramat was kept in the range of 10-500 μg·L-1, with detection limit (3S/N) of 0.75 μg·kg-1 and lower limit of determination (10S/N) of 2.51 μg·kg-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 79.8%-101%, with RSD's (n=6) in the range of 4.1%-8.7%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201708004
所属栏目 工作简报
基金项目 山东出入境检验检疫科研课题资助项目(SK201425)
收稿日期 2016/8/1
修改稿日期
网络出版日期
作者单位点击查看
备注郭庆龙(1981-),男,山东菏泽人,高级农艺师,硕士,主要从事植物检疫及食品安全分析工作,gql1235@163.com
引用该论文: GUO Qinglong,GUAN Xufang,ZHAO Yong,LI Ruijuan,YU Jianlei. GC-MS Determination of Residual Amount of Spirotetramat in Vegetables and Fruits[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2017, 53(8): 885~889
郭庆龙,管旭芳,赵勇,李瑞娟,于建垒. 气相色谱-质谱法测定蔬菜和水果中螺虫乙酯的残留量[J]. 理化检验-化学分册, 2017, 53(8): 885~889
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】刘长令.世界农药大全-杀虫剂卷[M].北京:化学工业出版社, 2012.
【2】杨吉春,吴峤,孙旭峰,等.杀虫、杀螨剂开发的新进展[J].农药, 2012,51(10):704-705.
【3】宋稳成,单炜力,简秋,等.国际食品法典农药残留限量标准最新动态及发展趋势[J].农药科学与管理, 2013,34(1):31-39.
【4】郑庆伟.加拿大拟修订稀禾定、2甲4氯和螺虫乙酯的最大残留限量[J].农药市场信息, 2013(28):42-42.
【5】MOHAPATRA S, DEEPA M, JAGADISH G K. An efficient analytical method for analysis of spirotetramat and its metabolite spirotetramat-enol by HPLC[J]. Bull Environ Contam Toxicol, 2012,88:124-128.
【6】ZHU Y L, LIU X G, XU J, et al. Simultaneous determination of spirotetramat and its four metabolitesin fruits and vegetables using a modified quick, easy, cheap, effective, rugged, and safe method and liquid chromatography/tandem mass spectrometry[J]. Journal of Chromatography A, 2013,1299:71-77.
【7】HAN Y T, XU J, DONG F S, et al. The fate of spirotetramat and its metabolite spirotetramat-enol in apple samples during apple cider processing[J]. Food Control, 2013,34(2):283-290.
【8】严会会,胡斌,刘惠民,等.高效液相色谱串联质谱法分析烟草中15种农药残留[J].烟草化学, 2011(7):43-47.
【9】田宏哲,杜芳,苑馨方,等.高效液相色谱法测定蔬菜中螺虫乙酯的残留[J].农药, 2015,54(4):289-291.
【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.
【2】杨吉春,吴峤,孙旭峰,等.杀虫、杀螨剂开发的新进展[J].农药, 2012,51(10):704-705.
【3】宋稳成,单炜力,简秋,等.国际食品法典农药残留限量标准最新动态及发展趋势[J].农药科学与管理, 2013,34(1):31-39.
【4】郑庆伟.加拿大拟修订稀禾定、2甲4氯和螺虫乙酯的最大残留限量[J].农药市场信息, 2013(28):42-42.
【5】MOHAPATRA S, DEEPA M, JAGADISH G K. An efficient analytical method for analysis of spirotetramat and its metabolite spirotetramat-enol by HPLC[J]. Bull Environ Contam Toxicol, 2012,88:124-128.
【6】ZHU Y L, LIU X G, XU J, et al. Simultaneous determination of spirotetramat and its four metabolitesin fruits and vegetables using a modified quick, easy, cheap, effective, rugged, and safe method and liquid chromatography/tandem mass spectrometry[J]. Journal of Chromatography A, 2013,1299:71-77.
【7】HAN Y T, XU J, DONG F S, et al. The fate of spirotetramat and its metabolite spirotetramat-enol in apple samples during apple cider processing[J]. Food Control, 2013,34(2):283-290.
【8】严会会,胡斌,刘惠民,等.高效液相色谱串联质谱法分析烟草中15种农药残留[J].烟草化学, 2011(7):43-47.
【9】田宏哲,杜芳,苑馨方,等.高效液相色谱法测定蔬菜中螺虫乙酯的残留[J].农药, 2015,54(4):289-291.
【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.
相关信息