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超声辅助提取-液相色谱-串联质谱法同时测定油料作物中6种新型乙酰乳酸合成酶抑制剂类除草剂残留
引用本文:杨欢,吴小亮,张函彤,何巧,倪妍霞,黄思琦,牟仁祥.超声辅助提取-液相色谱-串联质谱法同时测定油料作物中6种新型乙酰乳酸合成酶抑制剂类除草剂残留[J].色谱,2018,36(11):1132-1139.
作者姓名:杨欢  吴小亮  张函彤  何巧  倪妍霞  黄思琦  牟仁祥
作者单位:中国水稻研究所, 农业农村部稻米及制品质量监督检验测试中心, 农业农村部稻米产品质量安全风险评估实验室, 浙江 杭州 310006
基金项目:现代农业产业技术体系建设专项资金资助(CARS-01-47).
摘    要:将超声辅助提取与液相色谱-质谱联用技术相结合,建立了油料作物中6种新型乙酰乳酸合成酶(ALS)抑制剂类除草剂(甲基二磺隆、氯吡嘧磺、双草醚、嘧草醚、嘧苯胺磺隆和乙氧嘧磺隆)的痕量多残留检测技术。比较了超声辅助提取和QuEChERS提取2种方法对6种除草剂的提取回收率,并根据净化效果和吸附作用对十八烷基键合硅胶吸附剂(C18)、乙二胺-N-丙基硅烷(PSA)、石墨化炭黑(GCB)、弗罗里硅土(Florisil)和增强型基质去除吸附剂(EMR) 5种吸附材料进行优化。结果表明,超声辅助提取可使6种化合物的提取回收率在90. 0%以上,EMR对6种化合物的吸附作用较小,且可有效去除油脂干扰,减小基质效应。6种除草剂在0. 05~500. 0μg/L范围内具有良好的线性,相关系数均大于0. 998 4。该方法检出限和定量限分别为0. 08~0. 8μg/kg和0. 25~2. 5μg/kg。6种化合物在油菜籽、大豆、花生米和葵花籽4种基质中3个加标水平下的加标回收率为70. 7%~103. 8%,相对标准偏差为0. 8%~9. 2%,可应用于油料作物中6种ALS抑制剂类除草剂的同时测定。

关 键 词:液相色谱-串联质谱  超声辅助提取  增强型基质去除吸附剂  乙酰乳酸合成酶抑制剂类除草剂  油料作物
收稿时间:2018-06-21

Simultaneous determination of six novel acetolactate synthase inhibitor herbicide residues in oil crops based on ultrasound assisted extraction liquid chromatography-tandem mass spectrometry
YANG Huan,WU Xiaoliang,ZHANG Hantong,HE Qiao,NI Yanxia,HUANG Siqi,MOU Renxiang.Simultaneous determination of six novel acetolactate synthase inhibitor herbicide residues in oil crops based on ultrasound assisted extraction liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography,2018,36(11):1132-1139.
Authors:YANG Huan  WU Xiaoliang  ZHANG Hantong  HE Qiao  NI Yanxia  HUANG Siqi  MOU Renxiang
Affiliation:Rice Product Quality Inspection and Supervision Center, Ministry of Agriculture, Laboratory of Quality and Safety Risk Assessment for Rice, Ministry of Agriculture, China National Rice Research Institute, Hangzhou 310006, China
Abstract:Ultrasound-assisted extraction coupled with liquid chromatography-tandem mass spectrometry (UAE-LC-MS/MS) was used to develop a trace multi-residue detection method for six novel acetolactate synthase (ALS) inhibitor herbicide residues (mesosulfuron-methyl, halosulfuron-methyl, bispyribac-sodium, pyriminobac-methyl, orthosulfamuron, and ethoxysulfuron) in oil crops. In this study, the recoveries of the six herbicides based on ultrasound-assisted and QuEChERS extraction methods were compared, and five adsorbent materials (C18, PSA, GCB, Florisil, and EMR) were optimized based on their purification and adsorption capacities. The results showed that the ultrasound-assisted extractions gave recoveries greater than 90% for the six compounds. Furthermore, EMR showed little adsorption for the six compounds and a reduced matrix effect by effective removal of the oil lipids. The six herbicide residues had good linearities in the concentrations ranging from 0.05 to 500.0 μg/L, and the correlation coefficients were greater than 0.9984. The limits of detection and limits of quantification for this method were 0.08-0.8 μg/kg and 0.25-2.5 μg/kg, respectively. The recoveries of the six pesticides at three spiked levels in four matrices (rapeseed, soybean, peanut, and sunflower seed) ranged from 70.7% to 103.8%, with relative standard deviations of 0.8%-9.2%. This method was successfully applied to the simultaneous determination of six ALS inhibitor herbicide residues in oil crops.
Keywords:liquid chromatography-tandem mass spectrometry (LC-MS/MS)  ultrasound-assisted extraction (UAE)  enhanced matrix removal (EMR)  acetolactate synthase inhibitor herbicides  oil crops
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