液相色谱-质谱法检测油菜子、植株和土壤中三唑醇的残留

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。

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

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 ProElut 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％～l10％,and the relative standard deviation was lower than 10％.The limit of detectable amount(S/N=10) was 1.7×10-9 g.The accuracy and precision of this method can meet the determinate requirements.