低温提取气相色谱法测定大葱中辛硫磷
Extraction of Phoxim in Welsh Onion Under Low Temperature and Its Determination by Gas Chromatography
摘 要
建立了气相色谱法测定大葱中辛硫磷残留量的分析方法.大葱样品经冷冻后,采用约2 ℃乙腈提取,提取液盐析后浓缩供气相色谱分析.由于辛硫磷的热不稳定性,通过优化气相色谱条件,可减少热分解,提高响应值,辛硫磷的质量浓度在0.10~10.0 mg·L-1范围与峰面积呈线性关系(r=0.999 9),方法的检出限为0.01 mg·kg-1,在0.02~0.10 mg·kg-1添加水平回收率为83.1%~105.0%,相对标准偏差为2.6%~9.2%.
气相色谱法
辛硫磷
大葱
Extraction under low temperature
Gas chromatography
Phoxim
Welsh onion
Abstract
Residual phoxim in welsh onion was extracted with acetonitrile at about 2 ℃,and the extract was evaporated to nearly dryness after salting out with sodium chloride.The residue was taken up with 1 mL of acetone and was ready for GC determination.Considering the thermoinstability of phoxim,the conditions of gas-chromatography were optimized to reduce its thermo-decomposition and to raise response value.Linear relationship between the peak area and concentration of phoxim was kept in the range of 0.10-10.0 mg·L-1 (r=0.999 9),with its detection limit of 0.01 mg·kg-1.Recovery tests were made by addition of standard phoxim in the concentration range of 0.02 to 0.10 mg·kg-1,and the values of recovery obtained were in the range 88.1%-105.0%,and precision tests were also performed,giving values of RSD′s (n=6) in the range of 2.6%-9.2%.
中图分类号 O657.37
所属栏目 工作简报
基金项目
收稿日期 2007/1/13
修改稿日期
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备注王连珠(1966-),女,福建漳州人,工程师,从事食品卫生检验.
引用该论文: WANG Lian-zhu,HU Chao-yang,ZHENG Jun-chao,YOU Jun,WANG Rui-long,LIU Yi-na. Extraction of Phoxim in Welsh Onion Under Low Temperature and Its Determination by Gas Chromatography[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2007, 43(6): 447～449
王连珠,胡朝阳,郑俊超,游俊,王瑞龙,刘溢娜. 低温提取气相色谱法测定大葱中辛硫磷[J]. 理化检验－化学分册, 2007, 43(6): 447～449
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参考文献
【1】GB/T5009.102-2003植物性食品中辛硫磷农药残留量的测定[S]．
【2】NY/T761-2004蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留检测方法[S]．
【3】周瑶敏,王冬根,戴廷灿,等.用毛细管气相色谱法测定蔬菜中的辛硫磷[J].江西农业学报,2005,17(4):52-55．
【4】Satoru N,Ryouko S,Hiroshi K,et al.Analytical Method of Phoxim in Agricultural Products by GC-FPD and GC/MS(SIM)[J].Journal of the Food Hygienic Society of Japan,1995,36(2):233-243．
【5】周宏琛,王勇,闫秋成,等.高效液相色谱法测定大蒜中辛硫磷残留[J].食品科学,2006,27(6):192-194．
【6】王勇,周宏琛,闫秋成,等.高效液相色谱法测定浓缩胡萝卜汁中辛硫磷残留量[J].分析试验室,2006,25(6):81-83．
【7】李永新,孙成均,赵剑虹,等.高效液相色谱法同时测定蔬菜水果中的12种农药残留[J].色谱,2006,24(3):251-255．
【8】Guo Li,Liang Pei,Zhang Taozhi,et al.Use of Continuous-Flow Microextraction and Liquid Chromatography for Determination of Phoxim in Water Samples[J].Chromatographia,2005,61:523-526．
【9】Fernández M,Picó Y,Manes J.Simultaneous Determination of Carbamate and Organophosphorus Pesticides in Honeybees by Liquid Chromatography-Mass Spectrometry[J].Chromatographia,2003,58:151-158．
【10】王连珠,游俊,陈枝华,等.固相萃取-气相色谱法快速测定大葱中有机磷农药残留量[J].理化检验-化学分册,2005,41(12):880-883．
【11】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．
【12】王建华,张艺兵,汤志旭,等.微波处理-气相色谱法测定含硫蔬菜中的多类农药残留[J].分析测试学报,2005,24(1):100-102．
【13】黄志强,吴玉杰,马铭,等.低温提取气相色谱法测定荞头中13种有机磷农药残留量[J].分析科学学报,2006,22(1):46-48．
【2】NY/T761-2004蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留检测方法[S]．
【3】周瑶敏,王冬根,戴廷灿,等.用毛细管气相色谱法测定蔬菜中的辛硫磷[J].江西农业学报,2005,17(4):52-55．
【4】Satoru N,Ryouko S,Hiroshi K,et al.Analytical Method of Phoxim in Agricultural Products by GC-FPD and GC/MS(SIM)[J].Journal of the Food Hygienic Society of Japan,1995,36(2):233-243．
【5】周宏琛,王勇,闫秋成,等.高效液相色谱法测定大蒜中辛硫磷残留[J].食品科学,2006,27(6):192-194．
【6】王勇,周宏琛,闫秋成,等.高效液相色谱法测定浓缩胡萝卜汁中辛硫磷残留量[J].分析试验室,2006,25(6):81-83．
【7】李永新,孙成均,赵剑虹,等.高效液相色谱法同时测定蔬菜水果中的12种农药残留[J].色谱,2006,24(3):251-255．
【8】Guo Li,Liang Pei,Zhang Taozhi,et al.Use of Continuous-Flow Microextraction and Liquid Chromatography for Determination of Phoxim in Water Samples[J].Chromatographia,2005,61:523-526．
【9】Fernández M,Picó Y,Manes J.Simultaneous Determination of Carbamate and Organophosphorus Pesticides in Honeybees by Liquid Chromatography-Mass Spectrometry[J].Chromatographia,2003,58:151-158．
【10】王连珠,游俊,陈枝华,等.固相萃取-气相色谱法快速测定大葱中有机磷农药残留量[J].理化检验-化学分册,2005,41(12):880-883．
【11】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．
【12】王建华,张艺兵,汤志旭,等.微波处理-气相色谱法测定含硫蔬菜中的多类农药残留[J].分析测试学报,2005,24(1):100-102．
【13】黄志强,吴玉杰,马铭,等.低温提取气相色谱法测定荞头中13种有机磷农药残留量[J].分析科学学报,2006,22(1):46-48．
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