色谱

色谱 ›› 2012, Vol. 30 ›› Issue (11): 1203-1207.DOI: 10.3724/SP.J.1123.2012.06007

• 技术与应用 • 上一篇    

固相萃取-高效液相色谱-串联质谱法检测粮食及其制品中的呕吐毒素

黄娟1*, 陈国松2, 张晓燕1, 沈崇钰1, 吕辰2, 吴斌1, 刘艳1, 陈惠兰1, 丁涛1   

  1. 1. 江苏出入境检验检疫局动植物与食品检测中心, 江苏 南京 210001; 2. 南京工业大学理学院, 江苏 南京 210009
  • 收稿日期:2012-07-11 修回日期:2012-08-17 出版日期:2012-11-28 发布日期:2012-11-21
  • 通讯作者: 黄娟,工程师,主要从事食品中添加剂、抗生素、真菌毒素类的残留检测. Tel: (025)52345187, E-mail: huang-juan@yeah.net.
  • 基金资助:

    江苏检验检疫局科研项目(2010KJ32).

Determination of deoxynivalenol in grain and its products by solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry

HUANG Juan1*, CHEN Guosong2, ZHANG Xiaoyan1, SHEN Chongyu1, LV Chen2, WU Bin1, LIU Yan1, CHEN Huilan1, DING Tao1   

  1. 1. Animal, Plant and Food Inspection Center of Jiangsu Entry-Exit Inspection and Quarantine Bureau, Nanjing 210001, China; 2. College of Science, Nanjing University of Technology, Nanjing 210009, China
  • Received:2012-07-11 Revised:2012-08-17 Online:2012-11-28 Published:2012-11-21

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摘要： 建立了粮食及其制品中呕吐毒素的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品经乙腈-水(84:16, v/v)溶液提取,HLB固相萃取柱富集净化,采用HPLC-MS/MS法对目标物进行定性确证和定量分析。在Phenomenex Kinetex C18柱(100 mm×4.6 mm, 2.6 μm)上以0.3‰氨水和乙腈为流动相进行梯度洗脱分离;质谱模式为电喷雾负离子监测模式。本方法的检出限(以信噪比(S/N)=3计)和定量限(以S/N=10计)分别为20 μg/kg和50 μg/kg；在20～1000 μg/L范围内呈现良好的线性关系,相关系数(r)大于0.99。对本底空白的面粉、大麦、大豆、大米、玉米粉、木薯干、小麦等7种代表性基质进行50、100、500 μg/kg 3个含量水平的添加试验,回收率范围为75.6%～111.0%,精密度(以相对标准偏差(RSD)计)不大于13.0%。本方法准确可靠,灵敏度高,经济实用,可替代较为昂贵的免疫亲和柱和多功能净化柱,较大地降低检测成本。

关键词: 高效液相色谱-串联质谱, 固相萃取, 粮食, 粮食制品, 呕吐毒素

Abstract: A method was established for the determination of deoxynivalenol (vomitoxin) in grain and its products based on solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was firstly extracted by acetonitrile-water (84:16, v/v). The extract was then cleaned-up by an HLB solid phase extraction cartridge. The separation was carried out on a Phenomenex Kinetex C18 column (100 mm×4.6 mm, 2.6 μm) with a gradient elution using 0.3‰ ammonia solution-acetonitrile as mobile phases. The analysis of deoxynivalenol was performed under electrospray negative ionization mode. The limit of detection (LOD, S/N=3) and the limit of quantification (LOQ, S/N=10) were 20 μg/kg and 50 μg/kg, respectively. A good linearity (r ＞0.99) was achieved for the target compound over the range of 20~1000 μg/L. The recoveries at the three spiked levels (50, 100, 500 μg/kg) in the blank matrices such as flour, barley, soybean, rice, cornmeal, cassava and wheat, were varied from 75.6% to 111.0% with the relative standard deviations no more than 13.0%. The method is accurate, efficient, sensitive and practical. The cost of pretreatment is obviously reduced by replacing immunoaffinity columns and Mycosep columns with HLB columns which have the same purification effect.

Key words: deoxynivalenol, grain, grain products, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), solid-phase extraction (SPE)