摘要
建立了超高效液相色谱—串联质谱(UPLC-MS/MS)同时测定甜菜中4种不同类型长效除草剂(氯嘧磺隆、嗪草酮、莠去津、咪唑乙烟酸)残留量的分析方法。样品经过甲醇提取,C18前处理小柱净化处理,以BEH C18(50mm×2.1mm i.d.,1.7μm)为色谱柱,0.1%(v/v)甲酸水溶液-0.1%(v/v)甲酸乙腈溶液为流动相梯度洗脱,电喷雾电离,在多反应监测(MRM)模式下测定。该方法标准曲线的线性良好,R值均大于0.99。在添加水平在0.01mg/kg和0.1mg/kg条件下,4种除草剂回收率为72.1%～98.1%,相对标准偏差均小于10%,说明检测方法可靠。
A sensitive and specific UPLC-MS/MS has been developed for simultaneously analysis of four herbicides （e. g. , Imazethapyr, Chlorimuron-ethyl, Atrazine and Metribuzin） in sugarbeet so that these herbicides can be used reasonably. The herbicides residues were extracted from the sample by methanol, cleaned up by using of C18 SPE cartridge, and analyzed using UPLC-MS/MS in multiple reaction monitoring （MRM） modes with positive electrospray ionization. The analytical column was BEH C18 （50 mm×2.1 mm i. d. , 1. 7 μm） and the mobile phases were water containing 0. 1% （v/v） formic acid and acetonitrile containing 0. 1% （v/v） formic acid in gradient elution. The researching results show that the liner relationship between peak area and concentration was satisfactory, and the correlation coefficients（R） are all larger than 0. 99. The recoveries were between 72.1% and 98.1% at spiking levels of 0.01 mg/kg and 0. 1 mg/kg with the relative standard deviations （RSD） less than 10%.
出处
《黑龙江大学工程学报》
2013年第3期35-38,44,共5页
Journal of Engineering of Heilongjiang University
基金
黑龙江省教育厅科学技术研究项目(11541278)
