色谱

色谱

• 技术与应用 • 上一篇    

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

杨雯筌,沈伟健,赵增运,徐锦忠,沈崇钰,吴斌   

  1. Laboratory of Food, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China
  • 收稿日期:2007-10-11 修回日期:2007-12-29 出版日期:2008-07-30 发布日期:1983-12-25
  • 通讯作者: 沈伟健
  • 基金资助:
    “十一五”国家科技支撑计划项目(2006BAK02A08-8).

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

YANG Wenquan, SHEN Weijian, ZHAO Zengyun, XU Jinzhong, SHEN Chongyu, WU Bin   

  1. Laboratory of Food, Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China
  • Received:2007-10-11 Revised:2007-12-29 Online:2008-07-30 Published:1983-12-25
  • Contact: SHEN Weijian

PDF

625

被引次数

12

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0.005,0.01,0.02,0.04 mg/kg 4个加标水平下,环氟菌胺的平均回收率均处于74.9%～96.4%之间,相对标准偏差(RSD)小于9.7%。在10～1000ng/mL范围内线性关系良好,检出限为0.001 mg/kg,定量限为0.005 mg/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。

关键词: 负化学离子源, 固相萃取, 胡萝卜 , 环氟菌胺, 气相色谱-质谱联用

Abstract: 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 94.6% 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 1000 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.

Key words: carrot , cyflufenamid, gas chromatography-mass spectrometry (GC-MS), negative chemical ionization (NCI), solid phase extraction (SPE)