A selective and reliable method was developed and validated for the determination of 14 lipophilic pesticides in raw propolis by gas chromatography–tandem mass spectrometry (GC-MS/MS) analysis. A test portion of milled sample was extracted with n-hexane followed by back extraction with acetonitrile and cleanup using EMR-Lipid and Florisil column adsorption. Matrix-matched standards were used to compensate for matrix effects. Typical linear correlation coefficients (R²) were ≥ 0.989 in concentration range of 0.001–0.200 μg/mL. Method validation was carried out at three spiking levels and three individual days, and it was found that the mean interday average recoveries were 61.0–106.8% with relative standard deviations ≤ 16.9%. Limits of quantification were ranged from 0.002 to 0.020 μg/g. Analysis of market propolis samples showed contamination by pesticides (e.g., tau-fluvalinate) to some degree.

建立了一种选择性可靠的方法，并通过气相色谱-串联质谱（GC-MS / MS）分析法测定了蜂胶中14种亲脂性农药的有效性。研磨后的样品的测试部分用正己烷萃取，然后用乙腈反萃取，并使用EMR-Lipid和Florisil柱吸附进行净化。基质匹配的标准品用于补偿基质效应。典型的线性相关系数（R ²）在0.001-0.200μg/ mL的浓度范围内≥0.989。方法验证在三个加标水平和三个独立日内进行，发现平均日间平均回收率为61.0–106.8％，相对标准偏差≤16.9％。定量限为0.002至0.020μg/ g。对市场蜂胶样品的分析显示，农药（例如，tau-fluvalinate）在一定程度上受到污染。