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    QuEChERS提取-高效液相色谱-串联质谱法测定蔬菜中29种除草剂的残留量

    Determination of 29 Residual Herbicides in Vegetables by HPLC-MS/MS with QuEChERS Extraction

    • 摘要: 取匀浆后的蔬菜样品5.000 g,加入甲酸-乙腈(1+99)混合液10.0 mL,振荡提取20 min,加入氯化钠2.0 g,继续振荡20 min,离心5 min。分取上清液1.5 mL,加入由N-丙基乙二胺100 mg、十八烷基硅烷100 mg和自制的磁化碳纳米管10 mg混合组成的净化剂进行QuEChERS提取净化,混合物经0.22 μm滤膜过滤。滤液供高效液相色谱-串联质谱法分析。色谱分离中,选用Waters Cortects C18色谱柱为固定相,以不同比例组成的乙腈(A)和5 mmol·L-1乙酸铵溶液(B)的混合液为流动相进行梯度洗脱。洗脱液中29种除草剂的残留量按质谱条件进行测定。结果表明:29种除草剂的质量浓度均在5.0~40 μg·L-1范围内与对应的峰面积呈线性关系,检出限(3S/N)在0.5~1.5 μg·kg-1之间。以空白蔬菜样品为基体,用标准加入法进行回收试验,测得29种化合物的回收率在83.9%~99.7%之间,测定值的相对标准偏差(n=6)在1.3%~5.6%之间。

       

      Abstract: A portion of 5.000 g of the homogenized and pulpified vegetable sample was taken and extracted by shaking for 20 min with 10.0 mL of a mixture of formic acid and acetonitrile (1+99), 2.0 g of NaCl were added to the mixture and the shaking was continued for another 20 min. After centrifuging for 5 min, an aliquot of 1.5 mL of the supernatant was taken and purified by QuEChERS with a powder mixture containing 100 mg each of N-propyl ethylenediamine and octadecyl silane and 10 mg of self-prepared magnetized carbon nanotubes. The mixture was then filtered through 0.22 μm filtering membrane, and the filtrate was used for HPLC-MS/MS analysis. In the HPLC separation, Waters Cortects C18 column was selected as stationary phase and mixtures of CH3CN (A) and 5 mmol·L-1 CH3COONH4 solution (B) with various ratios were used as mobile phase in the gradient elution. Residual amounts of the 29 herbicides in the eluates were determined by MS/MS under the instrumental conditions. As shown by the results, linear relationships between values of peak area and mass concentration of the 29 herbicides in the range of 5.0-40 μg·L-1 were obtained, and the detection limits (3S/N) in the range of 0.5-1.5 μg·kg-1. Test for recovery by standard addition method was made using a blank vegetable sample as matrix, giving results in the range of 83.9%-99.7%, and RSDs (n=6) ranged from 1.3% to 5.6%.

       

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