高效液相色谱法测定粮谷中13种农药残留

Determination of 13 Pesticide Residues in Grains by HPLC

目的建立固相萃取-高效液相色谱法测定粮谷中13种农药残留的检测方法。方法样品用乙腈提取,利用CARB/NH2固相萃取柱净化,在C18色谱柱上,以乙腈-水溶液为流动相,采用梯度洗脱分离,二极管阵列(PDA)检测器多波长检测,外标法定量。结果在0.50 mg/L^10.0 mg/L范围内,13种农药的线性关系良好,方法的检出限为0.010 mg/kg^0.075 mg/kg,定量限为0.035 mg/kg^0.25 mg/kg。在高、中、低3个浓度水平的加标回收率为84.1%~115%,相对标准偏差(n=6)为1.4%~10.7%。结论该方法净化效果好,结果准确,适合于粮谷中13种农药残留的测定。

Objective To establish a method for determination of 13 pesticide residues in grains by solid phase extraction coupled with high performance liquid chromatography. Methods Analytes were extracted with acetonitrile purified by CARB/NH2 SPE separated on a C18 column （150 mm ×4.6 mm 3 μm） with gradient elution using acetonitrile-water as the mobile phase, and detected at multiple wavelengths using a photo diode array detector. Ouantification was performed by external standard method. Results Good linearity was obtained for 13 pesticide residues over the range of 0. 50 mg/L-10. 0 mg/L, the limits of detection were 0. 010 mg/kg 0. 075 mg/kg, and the limits of quantitation were 0. 035 mg/kg-0. 25 mg/kg. Spiked recoveries at three （ low, middle and high） concentration levels were 84. 1%-115% and the relative standard deviations （n =6） were 1.4%-10. 7%. Conclusion The proposed method has good purification effect and high accuracy, and is suitable for determination of 13 pesticide residues in grains.