液相色谱-质谱法检测油菜子、植株和土壤中三唑醇的残留  

Determination of Triadimenol Residue in Rapeseed,Plants and Soil by LC-MS

作　　者：刘军[1] 程云斌[1] 刘骞[1] 沈菁[1] 

机构地区：[1]湖北省农业科学院质量标准与检测技术研究所,武汉430064

出　　处：《湖北农业科学》2016年第22期5934-5936,5939,共4页Hubei Agricultural Sciences

基　　金：农业部农药检定所农药登记残留试验项目(2014F109)

摘　　要：建立液相色谱-质谱法检测油菜子、植株和土壤中三唑醇残留量的方法。油菜子和植株经乙腈提取,经Carbon/NH2柱净化,实现样品的制备;土壤则经乙腈提取浓缩后直接检测。在岛津VP-ODS色谱柱上,以乙腈＋0.1%甲酸水为流动相,梯度洗脱,采用电喷雾正离子（ESI＋）sim扫描离子模式,以m/z 296为定量检测离子。结果表明,三唑醇保留时间在11.9 min左右。在0.02～2.00 mg/L的浓度范围内呈良好的线性关系,其相关系数为0.999 7。在油菜子、植株、土壤中添加0.02、0.20、2.0 mg/kg 3个浓度的三唑醇标样,其回收率为71%～110%,相对标准偏差（n=5）均小于10%,最低检出量（S/N=10）为1.7×10-9 g。该方法准确度和精密度均能满足检测要求。A method for determination of triadimenol residue in rapeseed,plants and soil was established by LC-MS. Triadimenol residue was extracted from sample with acetonitrile,cleaned up by Pro Elut CARB / NH2 SPE to achieve sample preparation,and separatesd on the Shimadzu VP-ODS column,using a mixture of acetonitrile and 0.1% formic acid solution as mobile phase. Determination was made by using ESI and under the mode of SIM. Quectionantitative detection of ions at m / z 296,the retention time of pyraclostrobin was about 11.9 min. Linearity were held in the ranges of 0.02～2.00 mg / L with the correlation coefficient for 0.999 7. The average recoveries of triadimenol in rapeseed,plants and soil at the spiked amounts of 0.02～2.00 mg / kg were 71%～110%,and the relative standard deviation was lower than 10%. The limit of detectable amount（S/N=10） was1.7×10-9g. The accuracy and precision of this method can meet the determinate requirements.

关 键 词：三唑醇 残留 液相色谱-质谱 油菜子 土壤 

分 类 号：O657.63[理学—分析化学]