超高效液相色谱-串联质谱法测定面粉、玉米及其制品中的伏马菌素研究

山东大学学报(医学版) ›› 2012, Vol. 50 ›› Issue (4): 115-120.

超高效液相色谱-串联质谱法测定面粉、玉米及其制品中的伏马菌素研究

马皎洁1，胡骁2，邵兵3，林肖惠4，于红霞1，李凤琴4

1.山东大学公共卫生学院营养与食品卫生学教研室,济南 250012；
2.中国人民解放军武装警察部队后勤学院职业与环境危害生物标志物重点实验室，天津 300162；
3.北京市疾病预防控制中心，北京 100013；4.中国疾病预防控制中心营养与食品安全所，北京 100050

收稿日期:2011-12-13 出版日期:2012-04-10 发布日期:2012-04-10
通讯作者: 李凤琴(1963- )，研究员，博士生导师，主要从事食品微生物与风险评估方面的研究。 E-mail:lifengqin0224@gmail.com 于红霞(1955- )，教授，主要从事营养与食品卫生学方面的研究。 E-mail:yuhx@sdu.edu.cn
作者简介:马皎洁(1987- )，硕士研究生，主要从事营养与食品卫生学方面的研究。
基金资助:
国家质检总局公益项目(200910278)

Ultra performance liquid chromatography-tandem mass spectrometry
method for determination of fumonisins in wheat flour,
corn and corn-based products

MA Jiao-jie1, HU xiao2, SHAO Bing3, LIN Xiao-hui4, YU Hong-xia1 , LI Feng-qin4

1. Institute of Nutrition and Food Hygiene, School of Public Health, Shandong University, Jinan 250012, China;
2. Tianjin Key Laboratory for Biomarker of Occupational and Environmental Hazard, Logistics University of
Chinese People′s Armed Police Forces, Tianjin 300162, China;
3. Beijing CDC, Beijing 100013, China;
4. National Institute of Nutrition and Food Safety， China CDC, Beijing 100050, China

Received:2011-12-13 Online:2012-04-10 Published:2012-04-10

摘要/Abstract

摘要：

目的建立面粉、玉米及其制品中3种伏马菌素的超高效液相色谱-串联质谱(UPLCMS/MS)检测方法。方法样品用乙腈-水(50∶50, V/V)溶液提取，经MultiSep 211 净化柱富集净化后，用甲醇-甲酸(99∶1, V/V)溶液洗脱，洗脱液用UPLC-MS/MS进行测定。UPLC-MS/MS检测伏马菌素的条件为梯度洗脱，流动相为0.2%甲酸水和乙腈；质谱采集模式为电喷雾正离子多反应监测模式。结果 UPLC-MS/MS检测方法对3种伏马菌素的检出限均为0.2μg/kg，最低定量限为0.6μg/kg。不同加标水平的3种伏马菌素平均回收率为69.44%~114.69%。用所建方法对2011年甘肃及天津生产的39份玉米及30份面粉样品进行了分析，结果以伏马菌素B1的检出率最高，污染水平最为严重。结论 UPLC-MS/MS法具有操作简单、灵敏度高、重现性好等特点，可用于面粉、玉米及其制品中伏马菌素的检测。

关键词: 伏马菌素；面粉；玉米；超高效液相色谱-串联质谱

Abstract:

Objective To develop a solid-phase extraction method coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for determination of three fumonisins (fumonisin B1, fumonisin B2 and fumonisin B3) in wheat flour, corn and corn-based products． Methods The samples were extracted by 50%(V/V) acetonitrile-water, followed by cleaning up on a MultiSep 211 column. Three toxins were eluted by methanol-formic acid(99∶1, V/V) and analyzed by UPLC-MS/MS with gradient elution. Acetonitrile and 0.2%(V/V) formic acid-water were used as the mobile phases in the gradient elution． The mass spectrometric acquisitions were carried out by means of multiple reaction monitoring (MRM) in electrospray positive ionization mode． Results The limits of detection (LOD) and the limits of quantification (LOQ) for three fumonisins were 0.2μg/kg and 0.6μg/kg. The mean recoveries of three fumonisins at the different spiked levels ranged from 69.44% to 114.69%. 39 corn samples and 30 wheat flour samples collected from Gansu and Tianjin harvested in 2011 were analyzed with the developed method. Fumonisin B1 was the predominant toxin detected in terms of frequency and contamination level. Conclusion The developed method is simple， sensitive and reproducible，and meets the requirement for determination of the three fumonisins in wheat flour, corn and corn-based products．

Key words: Fumonisin; Wheat flour; Corn; Ultra performance liquid chromatographytandem mass spectrometry(UPLC-MS/MS)

中图分类号:

R155.5

马皎洁1，胡骁2，邵兵3，林肖惠4，于红霞1，李凤琴4. 超高效液相色谱-串联质谱法测定面粉、玉米及其制品中的伏马菌素研究[J]. 山东大学学报(医学版), 2012, 50(4): 115-120.

MA Jiao-jie1, HU xiao2, SHAO Bing3, LIN Xiao-hui4, YU Hong-xia1 , LI Feng-qin4. Ultra performance liquid chromatography-tandem mass spectrometry
method for determination of fumonisins in wheat flour,
corn and corn-based products[J]. JOURNAL OF SHANDONG UNIVERSITY (HEALTH SCIENCES), 2012, 50(4): 115-120.

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