MSPE—UPLC—MS/MS测定茶油中5种苯氧羧酸类除草剂残留

Determination of 5 phenoxyacid herbicides in camellia oil by magnetic solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

采用透射电镜、傅里叶红外光谱两种常见的纳米材料表征手段对合成的磁性石墨烯复合材料进行了表征,确认磁性石墨烯成功合成后,将其运用到茶油样品苯氧羧酸类除草剂残留分析前处理中,建立了茶油中5种苯氧羧酸类除草剂的磁固相萃取—超高效液相色谱—串联质谱快速分析方法。通过将磁性石墨烯在茶油中苯氧羧酸类除草剂检测中的运用,分析时间和分析成本都相对减少,并且提高了对目标化合物的吸附效率和洗脱效率。结果显示：5种苯氧羧酸类农药在0.01~0.20 mg/kg时,线性关系良好,相关系数均大于0.999 68;在0.02,0.05,0.10 mg/kg添加水平下,5种目标物的平均回收率为88.1%~95.0%,RSD为2.6%~7.3%,完全能够满足茶油中5种苯氧羧酸类农药的检测需要。

A magnetic graphene composite was prepared and characterized by transmission electron microscopy and fourier transform infrared spectroscopy. A novel method was developed for the simultaneous determination of 5 phenoxy acid herbicides in camellia oil by magnetic solid-phase extraction-ultra performance liquid chromatography-tandem mass spectrometry,which using magnetic graphene composite for enrichment and cleanup. The analysis time and cost of this method were relatively decreased by use of magnetic graphene in the detection of phenoxy acid herbicides in camellia oil,it also increased the efficiency of adsorption and elution of the target compounds. The result showed a good linear correlation with the coefficients greater than 0. 999 68 when the 5 phenoxy acid herbicides within the range from 0. 01 to 0. 20 mg / kg; the average recovery rate was from 88. 1% to 95. 0% with the relative standard deviation（ RSD）ranged from 2. 6% to 7. 3% when these 5 targets on the levels of 0. 02,0. 05,0. 10 mg / kg,which totally meet the testing needs of the 5 phenoxy acid pesticides in camellia oil.