固相萃取-高效液相色谱法测定水中痕量甲磺隆
SPE-HPLC Determination of Trace Amounts of Metsulfuron-Methyl in Water
摘 要
提出了高效液相色谱法测定水中痕量甲磺隆.水样经Oasis MCX固相萃取小柱富集并净化后,以Extend C18柱(250 mm×4.6 mm,5 μm)为固定相,0.2 mol·L-1甲酸-甲醇-乙腈(60+20+20)混合溶液为流动相进行分离,在225 nm波长处,用二极管阵列检测器测定.甲磺隆浓度在0.005~5.0 mg·L-1范围内与其峰面积呈线性关系,测定下限(10S/N)为0.005 mg·L-1.方法用于水样分析,加标回收率在94.0%~102.0%之间,相对标准偏差(n=6)小于6.5%.
固相萃取
甲磺隆
水
HPLC
Solid phase extraction
Metsulfuron-methyl
Water
Abstract
High performance liqiud chromatography with solid phase extraction was applied to the determination of residual amount of metsulfuron-methyl in water. The sample was enriched and purified by Oasis MCX SPE column. The eluate obtained was separated on Extend C18 column (250 mm×4.6 mm,5 μm),using a mixture of 0.2 mol·L-1 formic acid,methanol and acetonitrile mixed in the ratio of 60 to 20 to 20 (by volume) as mobile phase. DAD-detection at 225 nm was used in the determination. Linear relationship between values of peak area and mass concentration of metsulfuron-methyl was kept in the range of 0.005-5.0 mg·L-1. Lower limit of determination (10S/N) of the method was found to be 0.005 mg·L-1. On the base of water sample,test for recovery were made by standard addition method,values of recovery found were in the range of 94.0%-102.0%,and values of RSD′s (n=6)were less than 6.5%.
中图分类号 O652.63
所属栏目 工作简报
基金项目 浙江省自然科学基金项目(Y5080099);浙江省大型科学仪器设备协作共用平台科研计划项目(2008F7009)资助
收稿日期 2010/3/29
修改稿日期
网络出版日期
作者单位点击查看
备注施跃锦(1977-),男,浙江金华人,工程师,硕士,研究方向为废水治理.
引用该论文: SHI Yue-jin,CAI Mei-qiang. SPE-HPLC Determination of Trace Amounts of Metsulfuron-Methyl in Water[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(8): 923～925
施跃锦,蔡美强. 固相萃取-高效液相色谱法测定水中痕量甲磺隆[J]. 理化检验－化学分册, 2010, 46(8): 923～925
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】叶发兵,来欣,朱立红,等.除草剂绿磺隆和甲磺隆对后茬作物危害的研究[J].安徽农业科学,2006,34(1):86-88．
【2】HOLLAWAY K L,KOOKANA R S,MEQUINN D J,et al. Comparison of sulfonylurea herbicide residue detection in soil by bioassay,enzyme-linked immunosorbent assay and HPLC[J]. Weed Res,1999,39(2):383-397．
【3】ROUCHAUD J,NEUS O,COOLS K,et al. Flupyrsulfuron soil dissipation andmobility in winter wheat crops[J]. J Agric Chem,1999,47(9):3872-3878．
【4】张秀真,符素敏,高素莲,等.RP-HPLC内标法测定土壤中甲磺隆和氯磺隆的残留量[J].化学研究,2009,20(2):98-100．
【5】刘海燕,黄超.甲磺隆,氯磺隆,噻吩磺隆混剂液相色谱分析[J].农业科学与管理,2005,26(12):5-7．
【6】胡先文,叶发兵,董元彦.水中甲磺隆的气相色谱分析研究[J].光谱实验室,2003,20(4):547-549．
【7】金米聪,马建明,王立,等.尿液中杀鼠萘的固相萃取-高效液相色谱测定法[J].中华劳动卫生职业病杂志,2006,24(11):682-683．
【8】金米聪,马建明,陈晓红,等.饮用水中3种一氯酚异构体的液相色谱-质谱联用法测定研究[J].中国卫生检验杂志,2006,16(5):519-521．
【9】陈晓红,仇佩虹,李小平,等.固相萃取-高效液相色谱柱后衍生法测定水中痕量N-甲基氨基甲酸酯[J].中国卫生检验杂志,2006,16(1):9-11．
【10】李小平,蒋经伟,范建中,等.固相萃取HPLC法测定豆芽中4-氯苯氧乙酸钠[J].中国卫生检验杂志,2006,16(3):267-268,269．
【2】HOLLAWAY K L,KOOKANA R S,MEQUINN D J,et al. Comparison of sulfonylurea herbicide residue detection in soil by bioassay,enzyme-linked immunosorbent assay and HPLC[J]. Weed Res,1999,39(2):383-397．
【3】ROUCHAUD J,NEUS O,COOLS K,et al. Flupyrsulfuron soil dissipation andmobility in winter wheat crops[J]. J Agric Chem,1999,47(9):3872-3878．
【4】张秀真,符素敏,高素莲,等.RP-HPLC内标法测定土壤中甲磺隆和氯磺隆的残留量[J].化学研究,2009,20(2):98-100．
【5】刘海燕,黄超.甲磺隆,氯磺隆,噻吩磺隆混剂液相色谱分析[J].农业科学与管理,2005,26(12):5-7．
【6】胡先文,叶发兵,董元彦.水中甲磺隆的气相色谱分析研究[J].光谱实验室,2003,20(4):547-549．
【7】金米聪,马建明,王立,等.尿液中杀鼠萘的固相萃取-高效液相色谱测定法[J].中华劳动卫生职业病杂志,2006,24(11):682-683．
【8】金米聪,马建明,陈晓红,等.饮用水中3种一氯酚异构体的液相色谱-质谱联用法测定研究[J].中国卫生检验杂志,2006,16(5):519-521．
【9】陈晓红,仇佩虹,李小平,等.固相萃取-高效液相色谱柱后衍生法测定水中痕量N-甲基氨基甲酸酯[J].中国卫生检验杂志,2006,16(1):9-11．
【10】李小平,蒋经伟,范建中,等.固相萃取HPLC法测定豆芽中4-氯苯氧乙酸钠[J].中国卫生检验杂志,2006,16(3):267-268,269．
相关信息
