摘要
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.
出处
《色谱》
CAS
CSCD
北大核心
2008年第4期526-528,共3页
Chinese Journal of Chromatography
基金
"十一五"国家科技支撑计划项目(2006BAK02A08-8)
关键词
固相萃取
气相色谱-质谱联用
负化学离子源
环氟菌胺
胡萝卜
solid phase extraction (SPE)
gas chromatography-mass spectrometry (GC-MS)
negative chemical ionization (NCI)
cyflufenamid
carrot