液相色谱-串联四极杆质谱法测定鸡蛋中8种三唑类农药残留量

目的建立液相色谱-串联四极杆质谱法测定鸡蛋中丙环唑、三唑酮、烯唑醇、抑霉唑、三唑醇、戊唑醇、氟硅唑和三环唑残留量的分析方法。方法取均质后的鸡蛋样品经乙腈溶液提取,加入无水硫酸镁和氯化钠进行脱水和盐析,高速离心后,取适量上层提取液经0.1%(V:V)甲酸稀释后,用中性氧化铝粉末净化并以10000 r/min离心取上清液,过0.22μm滤膜后上机测定。使用反相色谱柱进行分离,流动相为0.1%甲酸与乙腈,采用梯度程序进行洗脱,串联四极杆质谱法进行定性定量分析。结果 8种农药在2.5~250μg/kg范围内线性关系良好(r≥0.995),方法的检出限为1μg/kg,定量限为2.5μg/kg,添加回收率在78.31%~88.53%内,相对标准偏差低于10%。结论该方法具有较好的准确度与精密度,适用于鸡蛋中丙环唑、三唑酮、烯唑醇、抑霉唑、三唑醇、戊唑醇、氟硅唑和三环唑的残留量测定。

Determination of 8 triazoles pesticide residues in eggs by liquid chromatography-triple quadrupole tandem mass spectrometry

Objective To establish a method for the determination of propiconazole, triadimefon, diniconazol, enilconazole, triadimenol, tebuconazol, flusilazole and tricyclazole residues in eggs by liquid chromatography-triple quadrupole tandem mass spectrometry. Methods Homogenized egg samples were extracted with acetonitrile, and dehydrated and salted out with anhydrous magnesium sulfate and sodium chloride. After high speed centrifugation, the extract was diluted by the 0.1%(V:V) formic acid and purified by the neutral alumina powder. After 10000 r/min centrifugation, the extract was filtered by 0.22 μm film and then detected. The target was separated by gradient elution with a reverse phase column as the stationary phase and 0.1% formic acid and acetonitrile as the mobile phase. Triple quadrupole tandem mass spectrometry was used for qualitative and quantitative analysis. Results Eight triazoles had good linear relationships in the range of 2.5-250 μg/kg, and the correlation coefficients were above 0.995. The limit of detection of the method was 1 μg/kg and the limit of quantitative was 2.5 μg/kg. The recoveries were between 78.31% and 88.53%, with the relative standard deviations(RSDs) were lower than 10%. Conclusion This method has good accuracy and precision, which is suitable for the determination of 8 triazoles residues in eggs.