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目的采用超高效合相色谱(UpC~2)-二极管阵列检测器(PDA)法快速分析土壤中啶虫咪的含量。方法在检测波长为254 nm条件下,通过对色谱柱,流动相,柱温以及QuEchERS前处理方式各个参数优化,最终确定色谱柱选择ACQUITY UPC~2 2-EP柱(3.0 mm×100 mm,1.7岬),柱温为70℃,背压为1600 psi,流动相为甲醇和超临界CO_2。同时分析实验过程中对样品含量测定的影响,分析该方法测定中的不确定度因素。结果经过分析,可以得出在0.002~2.0μg/mL线性范围内回收率良好,且最小检出限为0.002μg/kg,定量限为0.006μg/kg,线性方程为Y=37.5X-16.4,相关系数为0.9999,回收率在75%~105%之间,相对标准偏差低于10%。土壤中啶虫脒的实际测定不确定度为0.00030 mg/kg,k=2。结论使用超高效合相色谱能够准确、迅速地测定土壤中啶虫脒的含量。当土壤中啶虫脒的含量接近测定方法的最低限量时,需要参考检测方法的不确定度,并将其应用到最终结果的确定中,提高数据的准确性。
OBJECTIVE To rapidly analyze the contents of acetamiprid in soil by using UPC-2 (Diode Array Detector) method. Methods The parameters of column, mobile phase, column temperature and QuEchERS pretreatment were optimized at the detection wavelength of 254 nm. The column was finally selected for ACQUITY UPC ~ 2 2-EP column (3.0 mm × 100 mm, 1.7 Cape), column temperature of 70 ℃, back pressure of 1600 psi, the mobile phase of methanol and supercritical CO_2. At the same time, the influence of the determination of the sample content during the experiment is analyzed, and the uncertainty factors in the determination of the method are analyzed. The results showed that the recovery was good in the linear range of 0.002 ~ 2.0μg / mL with the minimum detectable limit of 0.002μg / kg, the limit of quantitation of 0.006μg / kg, the linear equation of Y = 37.5X-16.4, The correlation coefficient was 0.9999, the recovery was between 75% and 105%, and the relative standard deviation was less than 10%. The actual measured uncertainty of acetamiprid in soil is 0.00030 mg / kg, k = 2. Conclusion The determination of acetamiprid in soil can be performed accurately and rapidly using ultra-high performance gas chromatography. When the content of acetamiprid in the soil is close to the minimum of the determination method, the uncertainty of the detection method needs to be referred to and applied to the determination of the final result to improve the accuracy of the data.