气相色谱-负化学源质谱法测定蜂蜜和王浆中4种杀虫剂的残留

建立了气相色谱-负化学源质谱（GC-NCI/MS）测定蜂蜜和王浆中4种杀虫剂残留量的方法。蜂蜜样品由乙酸乙酯提取、乙二胺-N-丙基硅烷（PSA）净化，而王浆样品经乙腈-水（1：1，v/v）提取、C18固相萃取柱净化，采用GC-NCI/MS测定，外标法定量。结果表明：在50~500 μg/L范围内4种农药的线性良好；所有农药的LOD在0.12~5.0 μg/kg之间，LOQ在0.40~16.5 μg/kg之间；在10、15、20 μg/kg 3个添加水平下，4种农药的平均回收率在78.2%~110.0%之间，且RSD均小于14%。所有农药的测定均没有出现干扰峰。该方法简单、快速，准确度、精密度和选择性高，抗干扰能力强，可用于蜂蜜和王浆中这4种农药的快速检测。

Determination of four insecticide residues in honey and royal jelly by gas chromatography-negative chemical ionization mass spectrometry

A method was developed for the determination of four insecticide residues in honey and royal jelly by gas chromatography-negative chemical ionization mass spectrometry (GC-NCI/MS). The honey and royal jelly samples were treated with different preparation methods as the result of the different components. The honey sample was extracted with ethyl acetate and cleaned up with primary second amine, and the royal jelly sample was extracted with acetonitrile-water (1:1, v/v), and cleaned up with a C18 solid-phase extraction column. Finally, the extracts of the honey and royal jelly were analyzed by GC-NCI/MS in selected ion monitoring (SIM) mode separately. External standard calibration method was used for quantification. The linearities of calibration curves of the four insecticides were good with the correlation coefficients greater than 0.99 in the range of 50-500 μg/L. The limits of the detection (LODs) of the four insecticides were in the range of 0.12-5.0 μg/kg, and the limits of the quantification (LOQs) were in the range of 0.40-16.5 μg/kg. The recoveries of the four insecticides spiked in honey and royal jelly at three spiked levels (10, 15 and 20 μg/kg) were in the range of 78.2%-110.0%, and the relative standard deviations (RSDs) were all below 14%. The sensitivity and selectivity of this method were good with no interfering peaks. The proposed method is simple, quick and effective to analyze the four insecticide residues in honey and royal jelly.