作者：苟健1, 潘志明1, 余海洋2
作者单位：1. 德阳市产品质量监督检验所, 四川 德阳 618000;
2. 中国测试技术研究院, 四川 成都 610021
关键词：食用植物油;高效氟吡甲禾灵;吡氟甲禾灵;涡旋萃取;气相色谱-质谱联用仪
摘要：
为检测食用植物油中高效氟吡甲禾灵和吡氟甲禾灵残留量，以菜籽油、食用调和油为研究对象，建立食用植物油中高效氟吡甲禾灵和吡氟甲禾灵的气相色谱-质谱联用仪测定方法。样品经乙腈涡旋萃取，PAEs检测玻璃萃取管净化，用气相色谱-质谱联用仪测定，外标法定量。结果表明：高效氟吡甲禾灵和吡氟甲禾灵在10~5 000 g/L范围内具有良好的线性关系（r0.999 5），方法检出限分别为1.0，1.4 g/kg，定量限分别为3.3，4.5 g/kg。在20~1 000 g/kg的添加水平，高效氟吡甲禾灵和吡氟甲禾灵的回收率在95%~110%之间，方法精密度试验的相对标准偏差在5%以内。该方法适用于食用植物油中高效氟吡甲禾灵和吡氟甲禾灵的定性和定量测定。
Determination of haloxyfop-P-methyl and haloxyfop-ethoxyethyl in edible vegetable oils by gas chromatography-mass spectrometry
GOU Jian1, PAN Zhiming1, YU Haiyang2
1. Deyang Product Quality Supervision and Inspection Institute, Deyang 618000, China;
2. National Institute of Measurement and Testing Technology, Chengdu 610021, China
Abstract: For the detection of haloxyfop-P-methyl and haloxyfop-ethoxyethyl in edible vegetable oils, with rapeseed oil and edible blend oil as the object of the research, the method for determination of haloxyfop-P-methyl and haloxyfop-ethoxyethyl in edible vegetable oils was established by gas chromatography-mass spectrometry(GC-MS). The sample was extracted in acetonitrile by vortex extraction and purified by SPEs. GC-MS was used for determination with external standard method applied for quantification. The results show that in a range of 10-5 000 μg/L, haloxyfop-P-methyl and haloxyfop-ethoxyethyl have a good liner relationship(r>0.999 5) with method detection limit respectively being 1.0 μg/kg and 1.4 μg/kg and quantitation limit being 3.3 μg/kg and 4.5 μg/kg. Under the adding range of 20-1 000 μg/kg, the recovery rate ranges from 95% to 110% and relative standard deviation(RSD) of the precision test is within 5%. Thus the method is applicable to qualitative and quantitative determination of haloxyfop-P-methyl and haloxyfop-ethoxyethyl in edible vegetable oils.
Keywords: edible vegetable oils;haloxyfop-P-methyl;haloxyfop-ethoxyethyl;vortex extraction;GC-MS
2017, 43(9): 64-67,80 收稿日期: 2017-01-02;收到修改稿日期: 2017-03-09
基金项目:
作者简介: 苟健(1962-),男,四川德阳市人,工程师,主要从事食品检测与管理工作。
参考文献
[1] 除草剂高效氟吡甲禾灵(Haloxyfop-P-methyl)[J]. 山东农药信息,2008(6):40-40.
[2] 王迪轩. 蔬菜常用除草剂-氟吡甲禾灵的使用与注意事项[J]. 农药市场信息,2015(9):54-54.
[3] 朱海霞,翁华,程亮,等. L高效氟吡甲禾灵乳油对春油菜田野燕麦的防治效果[J]. 湖北农业科学,2013,52(14):3297-3298.
[4] 魏桂华,闫强,高兴贵. 108 g/L高效氟吡甲禾灵乳油防除大豆田杂草效果研究[J]. 现代农业科技,2015(4):131-131.
[5] 吴菊香,王宝亮,许曼琳,等. 48%灭草松水剂与10.8%高效氟吡甲禾灵乳油防除夏直播花生田杂草效果研究[J]. 现代农业科技,2015(4):127-130.
[6] 武秀停,赵静,吴加伦,等. 气相色谱法测定穿心莲及其土壤中高效氟吡甲禾灵残留[J]. 分析科学学报,2013,29(2):227-230.
[7] 谢勇波,周清明,龚道新,等. 高效液相色谱法测定土壤、烟草和油菜中高效氟吡甲禾灵残留[J]. 农药,2011,50(3):209-212.
[8] 卢晓蕊,许海东,杜洪淼,等. 超高效液相串联质谱法测定食用油中高效氟吡甲禾灵[J]. 粮油加工(电子版),2015(4):29-31.
[9] 刘慧,曹赵云,张利强,等. 分散固相萃取-液相色谱-串联质谱法测定农产品中吡氟甲禾灵[J]. 分析试验室,2011, 30(3):83-86.
[10] 张艳. 农药残留分析中不同提取溶剂的评价[J]. 甘肃农业科技,2006(9):28-29.
[11] 韩梅,侯雪. 气相色谱串联质谱法测定香菇中几种氨基甲酸酯农药残留量[J]. 中国测试,2013,39(1):52-55.
[12] 化学分析实验室中的职责和质量控制指南:SN/T 3590-2013[S]. 北京:中国质检出版社,2013.
