气相色谱法测定大豆中24种有机磷农药的残留量
GC Determination of Residual Amounts of 24 Organophosphorous Pesticides in Soybean
摘 要
提出了用气相色谱-火焰光度检测器(GC-FPD)测定大豆中24种有机磷农药残留量的方法.采用乙腈匀质提取大豆试样中残留的有机磷农药,提取液依次经C18固相萃取柱、活性炭固相萃取柱和硅胶固相萃取柱净化.淋出液用DB-1701石英毛细管柱进行分离,GC-FPD检测,外标法定量.方法的检出限在0.005~0.010 mg·kg-1之间.所测24种农药的标准加入回收率在60.7%~115.6%之间,相对标准偏差(n=6)为1.7%~11.1%.
火焰光度检测器
有机磷农药
均质提取
固相萃取
大豆
GC
Flame photometric detector
Organophosphorous pesticides
Homogeneous extraction
Solid phase extraction
Soybean
Abstract
Twenty four organophosphorous pesticides (OPP′s) as residues remained in soybean were determined by gas chromatography with flame photometric detector (FPD).The soybean sample was homogeneously extracted with acetonitrile,and the extract was purified by passing through C18 SPE column,active carbon SPE column and florisil SPE column in succession.DB-1701 elastic quartz capillary column was used for separation,and method of external standard was adopted in the GC-FPD determination.Detection limits for the 24 pesticides found were in the range from 0.005 to 0.010 mg·kg-1.Recovery and precision were tested and results of recovery obtained were in the range of 60.7%-115.6%,and values of RSD′s (n=6) were ranged from 1.7% to 11.1%.
中图分类号 O657.7
所属栏目 工作简报
基金项目 “十一·五国家科技支撑计划”课题
收稿日期 2009/6/21
修改稿日期
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备注左海根(1979-),男,湖南醴陵人,硕士,研究方向为食品安全检测.
引用该论文: ZUO Hai-gen,ZHAN Chun-rui,WU Cai-hua,LI Ru-kun,GUO Ping. GC Determination of Residual Amounts of 24 Organophosphorous Pesticides in Soybean[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(10): 1201～1204
左海根,占春瑞,伍彩花,李如坤,郭平. 气相色谱法测定大豆中24种有机磷农药的残留量[J]. 理化检验－化学分册, 2010, 46(10): 1201～1204
被引情况:
【1】唐吉旺,王建秀,袁列江,林 源,肖 泳,陈鹏飞, "气相色谱-串联质谱法测定茶叶中24种农药残留量",理化检验－化学分册 51, 1557-1561(2015)
【2】白国涛,张春艳,卢华卫,刘来俊,郑书展, "凝胶渗透色谱-气相色谱法测定葵花籽中55种有机磷农药残留量",理化检验－化学分册 49, 835-839(2013)
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参考文献
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【2】王明泰,牟峻,吴剑,等.GC-MS法测定粮谷及油料中55种有机磷农药残留量[J].分析试验室,2006,25(11):110-117．
【3】刘咏梅,王志华,储晓刚.凝胶渗透色谱净化-气相色谱分离同时测定糙米中50种有机磷农药残留[J].分析化学,2006,34(6):808-810．
【4】朱晓兰,蔡继宝,杨俊,等.加速溶剂萃取-气相色谱法测定土壤中的有机磷农药残留[J].分析化学,2005,33(6):821-824．
【5】梅文泉,黎其万,黄司思,等.加热处理-气相色谱法测定韭菜中有机磷农药残留量[J].分析试验室,2006,25(8):42-44．
【6】汤富彬,陈宗懋,罗逢健,等.固相萃取-气相色谱法检测茶叶中的有机磷农药残留量[J].分析试验室,2007,26(2):43-47．
【7】胡小钟,储晓刚,余建新,等.气相色谱-质谱法快速筛选测定浓缩苹果汁中105种农药残留量[J].分析测试学报,2003,22(6):26-31．
【8】万益群,李艳霞.气相色谱-质谱法同时测定中药中有机磷和有机氮农药残留量[J].分析测试学报,2005,24(5):90-94．
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