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  

Simultaneous determination of six novel acetolactate synthase inhibitor herbicide residues in oil crops based on ultrasound assisted extraction liquid chromatography-tandem mass spectrometry

作　　者：杨欢[1] 吴小亮[1] 张函彤 何巧[1] 倪妍霞 黄思琦 牟仁祥[1] YANG Huan;WU Xiaoliang;ZHANG Hantong;HE Qiao;NI Yanxia;HUANG Siqi;MOU Renxiang(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)

机构地区：[1]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

出　　处：《色谱》2018年第11期1132-1139,共8页Chinese Journal of Chromatography

基　　金：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。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 500.0μg/L,and the correlation coefficients were greater than 0.998 4.The limits of detection and limits of quantification for this method were 0.08-0.8μg/kg and 0.25-2.5μg/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.

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 

分 类 号：O658[理学—分析化学]