SIMULTANEOUS DETERMINATION OF RESIDUAL AMOUNTS OF CHLORPYRIFOS CYPERMETHRIN AND FENVALERATE IN VEGETABLES BY GAS CHROMATOGRAPHY
摘 要
建立了气相色谱法同时测定蔬菜中毒死蜱、氯氰菊酯和氰戊菊酯残留量的分析方法.采用HP-5石英毛细管柱(30 m×0.25 mm,0.25 μm)和电子捕获检测器测定,用3种农药的基准物质配成混合标准溶液制作浓度范围在0.02~0.20 mg·L-1之间的校正曲线,3条曲线的相关系数分别为0.999 4,0.999 4和0.998 9.样品加标回收率为85.3%~93.1%,相对标准偏差为0.13%~2.16%,检出限分别为0.001,0.002和0.002 mg·kg-1.
Abstract
Gas chromatography was applied to the simultaneous determination of 3 pesticides,i.e.chlorpyrifos,cypermethrin and fenvalerate,in vegetables,and HP-5 quartz capillary column (30 m×0.25 mm i.d.×0.25 μm) and electron capture detector (ECD) were used in the separation and detection.Chromatographic parameters were described in detail.It was found that better efficiency of extraction and higher recovery were obtained by using petroleum ether as extractant than by using mixed solvents as extractant;and that the efficiency of purification was quite satisfactory by the use of the floridin silicious clay.A mixed standard solution was prepared from primary standards of the 3 pesticides,and calibration curve for each of the 3 pesticides was prepared covering the concentration ranges of 0.02 to 0.20 mg·L-1.The correlation coefficients of these calibration curves were 0999 for chlorpyrifos and cypermethrin,and 0.998 for fenvalerate;and their detection limits were 0.001,0.002 and 0.002 mg·kg-1 respectively.Recovery tests by addition of standard solutions at 3 concentration levels on the base of blank vegetable samples gave results in the range of 85.3% to 93.1%,and RSD′s obtained were in the range of 0.13% to 2.16%.
中图分类号 O657.37
所属栏目 工作简报
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收稿日期 2005/5/8
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备注陆勋元(1971-),男,浙江德清人,助理工程师,研究方向为分析化学.
引用该论文: LU Xun-yuan,JIANG Yong-xiang. SIMULTANEOUS DETERMINATION OF RESIDUAL AMOUNTS OF CHLORPYRIFOS CYPERMETHRIN AND FENVALERATE IN VEGETABLES BY GAS CHROMATOGRAPHY[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2006, 42(9): 737~739
陆勋元,蒋永祥. 气相色谱法同时检测和分析蔬菜中毒死蜱、氯氰菊酯和氰戊菊酯的残留量[J]. 理化检验-化学分册, 2006, 42(9): 737~739
被引情况:
【1】徐霞,朱智伟,应兴华, "西兰花中13种有机含磷农药在不同色谱柱上的色谱保留行为",理化检验-化学分册 48, 803-806(2012)
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参考文献
【1】GB/T 17332-1998,食品中有机氯和拟除虫菊酯类农药多种残留的测定[S].
【2】刘绍仁,叶纪明,姜淑秀,等.毒死蜱气相色谱分析方法的研究[J].农药,1992,31(2):29-30.
【3】汪军.GC-MS定性定量分析出口西兰花样品中毒死蜱的农药残留量[J].现代农药,2002(1):23-24.
【4】于生棣,于永庆,秦国宏,等.氯氰菊酯的气相色谱分析[J].农药,1992,31(2):41-42.
【5】朱九生,乔雄梧,秦曙,等.固相萃取净化气相色谱法快速测定土壤中的氯氰菊酯残留[J].环境化学,1997,16(2):116-118.
【6】杨长志,李淑琪,康庆贺,等.气相色谱法测定甜玉米中的氯氰菊酯﹑氰戊菊酯的残留[J].色谱,2003,21(5):531-533.
【7】徐爱平,王富华,赖穗春,等.果蔬中5种农药的同时检测与残留量分析[J].华中农业大学学报,2003,22(6):561-563.
【2】刘绍仁,叶纪明,姜淑秀,等.毒死蜱气相色谱分析方法的研究[J].农药,1992,31(2):29-30.
【3】汪军.GC-MS定性定量分析出口西兰花样品中毒死蜱的农药残留量[J].现代农药,2002(1):23-24.
【4】于生棣,于永庆,秦国宏,等.氯氰菊酯的气相色谱分析[J].农药,1992,31(2):41-42.
【5】朱九生,乔雄梧,秦曙,等.固相萃取净化气相色谱法快速测定土壤中的氯氰菊酯残留[J].环境化学,1997,16(2):116-118.
【6】杨长志,李淑琪,康庆贺,等.气相色谱法测定甜玉米中的氯氰菊酯﹑氰戊菊酯的残留[J].色谱,2003,21(5):531-533.
【7】徐爱平,王富华,赖穗春,等.果蔬中5种农药的同时检测与残留量分析[J].华中农业大学学报,2003,22(6):561-563.
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