| 孟冰冰,于洪春.QuEchERS-超高效合相色谱测定土壤中啶虫咪的含量及不确定度分析[J].食品安全质量检测学报,2016,7(5):2097-2104 |
| QuEchERS-超高效合相色谱测定土壤中啶虫咪的含量及不确定度分析 |
| Determination of acetamiprid content and analysis of uncertainty in the soil by QuEchERS-ultra performance convergence chromatography |
| 投稿时间：2015-12-08 修订日期：2016-02-26 |
| DOI： |
| 中文关键词: 超高效合相色谱 啶虫咪 不确定度评价 |
| 英文关键词:ultra performance convergence chromatography acetamiprid uncertainty evaluation |
| 基金项目:国家公益性行业(农业)科研专项(201003025)、现代农业产业技术体系建设专项资金(CARS-04) |
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| 中文摘要: |
| 目的 采用超高效合相色谱(UPC2)-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 UPC2 2-EP柱(3.0 mm×100 mm, 1.7 μm), 柱温为70 ℃, 背压为1600 psi,流动相为甲醇和超临界CO2。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0.002~2.0 μg/mL线性范围内回收率良好, 且最小检出限为0.002 μg/kg, 定量限为0.006 μg/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。 |
| 英文摘要: |
| Objective To establish a method for the rapid determination of acetamiprid in the soil by ultra performance convergence chromatography- photo-diode array (UPC2-PDA). Methods At the wavelength of 254 nm, single factor experiments were carried out to optimize the parameters, including chromatographic column, mobile phase, column temperature, pressure and QuEchERS. Finally, the chromatographic column was ACQUITY UPC2 2-EP (3.0 mm×100 mm, 1.7 μm), the column temperature was 70 ℃, the backpressure was 1600 psi, and the mobile phase was identified methanol and supercritical CO2. At the same time, the influence of the sample content was analyzed, and the uncertainty factors in the determination were analyzed. Results Under the optimum conditions, the calibration curve had a linearity in the range of 0.002~2.0 μg/mL with a correlation coefficient of 0.9999, the linear equation was Y=37.5X?16.4, the recoveries were in the range of 75%~105%, and the relative standard deviation were less than 10%. The limit of detection and limit of quantification were 0.002 μg/kg and 0.006 μg/kg, respectively. The actual measurement uncertainty of acetamiprid in the soil was 0.00030 mg/kg, k=2. Conclusion The use of UPC2 can accurately and rapidly determination of acetamiprid in the soil. It needs to reference the uncertainty of the detection method, and apply it to the final result determination for improving the accuracy of the data, when the content of acetamiprid in the soil was close to the lower limit of the detection method. |
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