气相色谱-负化学离子源质谱法检测胡萝卜中残留的环氟菌胺

Determination of cyflufenamid residue in carrots by gas chromatography-negative chemical ionization mass spectrometry

建立了胡萝卜中环氟菌胺残留量的气相色谱．负化学离子源质谱（GC—NCI／MS）检测方法。用乙酸乙酯对胡萝卜中的环氟菌胺进行提取，并经固相萃取（SPE）净化后，由GC—NCI／MS在选择离子监测模式（SIM）下测定。该方法的准确度和精密度较高，在0．005，0．01，0．02，0．04mg／kg 4个加标水平下，环氟菌胺的平均回收率均处于74．996～96．4％之间，相对标准偏差（RSD）小于9．796。在10～1000ng／mL范围内线性关系良好，检出限为0．001mg／kg，定量限为0．005mg／kg。该方法选择性好，抗干扰能力强，可作为胡萝卜中环氟菌胺残留检测的确证方法。

A method was developed for the determination of cyflufenamid residue in carrots by solid phase extraction-gas chromatography-negative chemical ionization mass spectrometry （SPE-GC-NCI/MS）. Cyflufenamid residue was extracted with ethyl acetate from carrots. The extract was cleaned-up by an active carbon SPE column connected to a neutral alumina SPE column. The analysis was carried out by the GC-NCI/MS with selected ion monitoring mode. The recoveries of cyflufenamid in carrot samples were in the range from 74.9% to 94.5% at four spiked levels, 0. 005, 0.01, 0.02, 0.04 mg/kg, and the relative standard deviations （RSD） were less than 9.7% for inter-days. The linearity of the method was good in the range from 10 to 1 000 ng/mL, and the limit of detection （LOD） was 0. 001 mg/kg, and the limit of quantitation （LOQ） was 0. 005 mg/kg. The method is selective without interference and is suitable for the determination and confirmation of cyflufenamid residue in carrots.