HPLC Simultaneous Determination of Residual Amounts of Pesticides in Fruits and Vegetables with Solid Phase Extraction
摘 要
提出了同时测定蔬菜、水果中9种农药残留的高效液相色谱分析方法.样品经乙腈超声提取及Florisil固相萃取柱富集,用正己烷-二氯甲烷(40+60)混合溶剂从柱上洗脱农药残留使净化.洗脱液在40 ℃氮气吹干,残渣用1.0 mL甲醇溶解,取1 μL样品溶液注入高效液相色谱仪测定.采用C18色谱柱分离,以甲醇-水混合溶液为流动相,紫外254 nm检测.结果表明:9种农药的质量浓度在0.01~1.0 mg·L-1范围内呈线性关系,方法的检出限(3S/N)在0.009~0.049 mg·kg-1之间.分别以蔬菜和水果为基体,加入标准溶液进行回收试验,测得蔬菜中9种农药的回收率为68.3%~103.2%,相对标准偏差(n=6)为1.8%~13.9%;水果中农药的回收率为69.4%~106.0%,相对标准偏差(n=6)为2.9%~11.8%.
Abstract
A method of HPLC for simultaneous determination of 9 kinds of pesticides in fruit and vegetable samples was proposed.The samples were extracted with acetonitrile,and residual pesticides in sample solution were separated and enriched by solid phase extraction (SPE) on Florisil column.The SPE column was eluted with a mixture of n-hexane and dichloromethane (40+60),and the eluate obtained was evaporated to dryness by N2-blowing at 40 ℃ and taken up with 1.0 mL of CH3OH.A aliquot of 1.0 μL was used for HPLC determination.C18 column was used as the stationary phase and a mixture of methanol and water was used as the mobile phase.UV detection at 254 nm was adopted.Linear relationships were found in the same range of 0.01-1.0 mg·L-1 for the 9 pesticides,with values of detection limit (3S/N) in the range of 0.009-0.049 mg·kg-1.On the base of samples of fruit and vegetable,test for recovery were made by standard adiition method.Values of recovery and RSD′s (n=6) found were in the ranges of 68.3%-103.2% and 1.8%-13.9% (for vegetables);69.4%-106.0% and 2.9%-11.8% (for fruits),respectively.
中图分类号 O657.63
所属栏目 工作简报
基金项目 云南省农药检定所农药分析方法研究课题
收稿日期 2009/4/2
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备注马莉莉(1979-),女,云南人,硕士生,主要从事现代仪器分析的研究.
引用该论文: MA Li-li,ZHANG Cheng-cong,WU Xiao-bo,QU Tian-yao. HPLC Simultaneous Determination of Residual Amounts of Pesticides in Fruits and Vegetables with Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(7): 825~828
马莉莉,张承聪,吴晓波,屈天尧. 固相萃取-高效液相色谱法同时测定果蔬中9种农药残留[J]. 理化检验-化学分册, 2010, 46(7): 825~828
被引情况:
【1】时磊,陈海英,蔡小虎,胡璟珂,吕爱娟,沈小明,孙艳艳, "超声提取-气相色谱法同时测定稻谷中18种有机氯农药和7种多氯联苯",理化检验-化学分册 52, 1090-1094(2016)
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参考文献
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【2】陈浩,王豹,韦明元,等.SPE-GC在水果和蔬菜有机磷农药残留分析中的应用[J].食品科学,2004,25(10):235-236.
【3】吴丽华,李建科,伍小红.气相色谱法测定苹果中的多种农药残留量[J].分析试验室,2006,25(11):46-50.
【4】李胜清,田华,柳训才,等.固相萃取-气相色谱法用于蔬菜中拟除虫菊酯类农药残留的检测研究[J].分析科学学报,2005,21(3):289-291.
【5】李云飞,彭云霞,张承聪.气相色谱-质谱联用仪测定果蔬中12种农药残留量[J].云南大学学报:自然科学版,2004,26:176-180.
【6】许泓,林安清,古珑,等.果蔬中107种残留农药的气相色谱-质谱检测方法[J].分析测试学报,2004,23(3):34-38.
【7】陶宏亮,关燕萍,苏晓峰,等.SPE-HPLC用于蔬菜中甲基对硫磷和对硫磷同时测定[J].华中农业大学学报,2006,25(1):46-49.
【8】MOLINA C,HONING M,BARCELO D.Determination of organophosphorous pesticides in water by SPE followed by LC/high flow pneumatically assisted electrospray MS[J].Anal Chem,1994,66(24):4444-4449.
【9】黄玉兰,马海燕,吴平谷.市售蔬菜中有机磷、拟除虫菊酯类农药残留量的测定和分析[J].中国公共卫生,1999,15(9):815.
【10】董顺玲,胡家炽,何志强,等.中药材中氨基甲酸酯类农药残留量的反相高效液相色谱法[J].药物分析杂志,2002,22(3):178-182.
【11】陶传江,郑姗姗,刘伟,等.蔬菜样本柱层析净化方法研究[J].农药科学与管理,2001,22(2):18-20.
【12】王龙根.蔬菜中6种菊酯农药残留的检测[J].安徽农业科学,2004,32(1):91-92.
【13】刘永波,贾立华,牛淑妍.气-质联用快速检测蔬菜、水果中农药多残留的分析方法[J].青岛科技大学学报:自然科学版,2003,24(6):491.
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