GC Determination of Residual Amount of Methamidophos in Tea with Solid Phase Extraction
摘 要
茶叶样品经乙酸乙酯提取,上清液于50 ℃蒸发至近干,加入乙酸乙酯溶解残渣后,经硅胶-石墨化碳混合柱净化。先以乙酸乙酯洗脱去除杂质,再以碱化乙腈洗脱并收集流出液,在50 ℃蒸发至近干,加乙酸乙酯定容至1 mL,供气相色谱分析。采用DB-1701色谱柱分离和火焰光度检测器检测,所得甲胺磷的线性范围为0.010~1.00 mg·L-1,方法的检出限(3S/N)为0.005 mg·kg-1。在0.010,0.020,0.080 mg·kg-1 3个浓度水平下进行回收试验,甲胺磷的回收率在85.0%~90.9%之间,相对标准偏差(n=6)在2.2%~4.3%之间。
Abstract
Sample of tea was extracted with ethyl acetate, and the supernatant was taken and evaporated to near dryness at 50 ℃. The residue was dissolved with ethyl acetate, and purified by passing through a column packed with silica gel and graphitized carbon. The column was washed with ethyl acetate to remove impurities, and then eluted the analyte with alkalified acetonitrile. The eluate obtained was evaporated to near dryness at 50 ℃, and taken up with 1 mL of ethyl acetate and used for GC analysis using the DB-1701 chromatographic column for separation and FPD for detection. Linearity range of methamidophos was kept between 0.010-1.00 mg·L-1, with detection limit (3S/N) of 0.005 mg·kg-1. Tests for recovery and precision were made by addition of 0.010, 0.020, 0.080 mg·kg-1 of standard solution, and analyzed by the proposed method, giving values of recovery in the range of 85.0%-90.9% and values of RSD′s (n=6) in the range of 2.2%-4.3% respectively.
中图分类号 O657.7
所属栏目 试验与研究
基金项目 福建出入境检验检疫局科技项目(FK201161)
收稿日期 2011/5/21
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联系人作者丁立平(43548624@qq.com)
备注丁立平(1980-),男,江西丰城人,硕士,工程师,主要从事进出口食品中农药、兽药残留检测。
引用该论文: DING Li-ping. GC Determination of Residual Amount of Methamidophos in Tea with Solid Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(7): 756~759
丁立平. 固相萃取-气相色谱法测定茶叶中甲胺磷残留量[J]. 理化检验-化学分册, 2012, 48(7): 756~759
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参考文献
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【3】PANG Guo-fang, FAN Chun-lin, LIU Y M, et al. Determination of residues of 446 pesticides in fruits and vegetables by three-cartridge solid-phase extraction-gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry[J]. J AOAC Int, 2006,89(3):740-741.PANG Guo-fang, FAN Chun-lin, ZHANG Feng, et al. High-throughput GC/MS and HPLC/MS/MS techniques for the multiclass, multiresidue determination of 653 pesticides and chemical pollutants in tea[J]. J AOAC Int, 2011,94(4):1253-1296.
【4】DARINKA S, LUCIJA Z. Multiresidue method for determination of 90 pesticides in fresh fruits and vegetables using solid-phase extraction and gas chromatography-mass spectrometry[J]. J Chromatogr A, 2003,1015(1):185-198.
【5】ZHANG H, CHEN Z L, YANG G S, et al. Microwave pretreatment and gas chromatography-mass spectrometry determination of herbicide residues in onion[J]. Food Chemistry, 2008,108(1):322-328.
【6】纪淑娟,刘长江,佐藤元昭,等.用气-质联用技术检测葱、蒜、韭菜中多种农药残留量时试样预处理方法[J].理化检验-化学分册, 2006,42(11):914-917.
【7】苏建峰,张金虎,林永辉,等.正相硅胶/选择洗脱-气相色谱法、液相色谱-质谱法检测食品中甲胺磷残留及其作用机理研究[J].分析化学, 2009,37(10):1426-1432.
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