固相萃取-气相色谱串联质谱法测定肉及肉制品中11种农药残留

Determination of eleven kinds of pesticide residues in meat and meat products by solid-phase extraction with gas chromatography tandem mass spectrometry

中文关键词:  气相色谱质谱联用  农药残留  肉及肉制品

英文关键词:gas chromatography-mass spectrometry  pesticide residues  meat and meat products

中文摘要:

      目的 建立固相萃取结合气相色谱串联质谱法同时测定肉及肉制品中11种常用农药的残留检测方法。方法 用乙腈提取肉及肉制品样品中残留农药, 经冷冻离心及PSA/Silica固相萃取柱净化后, 采用气相色谱-质谱联用法(gas chromatography tandem mass spectrometry, GC-MS)进行分析检测, 用内标标准曲线法定量。结果 11种农药在0.05~2.00 μg/mL浓度区间内线性方程的相关系数均大于0.9950, 检出限为0.002~ 0.020 mg/kg, 定量限为0.005~0.060 mg/kg。在样品中添加0.05、0.10、0.20 mg/kg 3个浓度水平的加标实验中, 样品的加标回收率为74.3%~118%, 相对标准偏差为2.1%~9.6%。结论 该方法的灵敏度、重复性和稳定性较高, 适用于肉及肉制品中11种农药残留的检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of 11 kinds of common pesticide residues in the meat and meat products by solid-phase extraction combined with gas chromatography -mass spectrometry (GC-MS). Methods The residual pesticides in meat and meat products were extracted by acetonitrile, purified by freeze centrifugation and PSA/silica solid-phase extraction column, and detected by GC-MS. The Internal standard calibration curves were used for quantitative analysis. Results The correlation coefficients of the linear equations of the eleven kinds of pesticide residues in the concentration range of 0.05?2.00 μg/mL were more than 0.9950, the detection limits range were 0.002?0.020 mg/kg, and the limits of quantitation were 0.005?0.060 mg/kg. In the spiked experiments with the addition of 0.05, 0.10, 0.20 mg/kg in the sample, the recoveries of standard addition of the sample were 74.3%?118%, and the relative standards deviation were 2.1%?9.6%. Conclusion The method has high sensitivity, repeatability and stability, and is suitable for the detection of 11 kinds of pesticide residues in meat and meat products.