色谱

色谱 ›› 2019, Vol. 37 ›› Issue (9): 963-968.DOI: 10.3724/SP.J.1123.2019.03014

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法快速测定六神曲中的米酵菌酸

王俊虎, 乔勇升, 王建, 朱渊   

  1. 泰州市食品药品检验所, 江苏 泰州 225300
  • 收稿日期:2019-03-12 出版日期:2019-09-08 发布日期:2015-07-30
  • 通讯作者: 朱渊
  • 基金资助:
    江苏省食品药品监督管理局科研项目（20170227）；泰州市科技支撑计划社会发展项目（TS201812）.

Rapid determination of bongkrekic acid in Liushenqu by ultra performance liquid chromatography-tandem mass spectrometry

WANG Junhu, QIAO Yongsheng, WANG Jian, ZHU Yuan   

  1. Taizhou Institute for Food and Drug Control, Taizhou 225300, China
  • Received:2019-03-12 Online:2019-09-08 Published:2015-07-30
  • Supported by:
    Scientific Research Project of Food and Drug Administration of Jiangsu Province of China (No. 20170227); Taizhou Science and Technology Support Program Social Development Project of China (No. TS201812).

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摘要： 基于超高效液相色谱-串联质谱法（UPLC-MS/MS），建立了快速测定六神曲中生物毒素米酵菌酸残留的检测方法。样品首先以甲醇作为提取溶剂进行超声提取，再用氨水调节pH值至8，过滤，滤液用Oasis MAX强阴离子交换固相萃取柱处理。采用Waters HSS T3色谱柱（100 mm×2.1 mm，1.8 μm）分离，以乙腈-含0.1%（体积分数）甲酸的10 mmoL/L甲酸铵溶液为流动相，采用电喷雾电离（ESI）源电离，电离模式为负离子模式，质谱检测模式为多反应监测（MRM）模式。在最佳条件下，米酵菌酸在0.5~100 μg/L范围内呈良好的线性关系，相关系数（R2）>0.99。方法的加标回收率为80.6%~85.3%，日内和日间精密度分别为4.2%~6.8%和8.2%~13.2%。方法的检出限（LOD，S/N=3）和定量限（LOQ，S/N=10）分别为0.4 μg/kg和1.2 μg/kg。实际样品测定中发现了六神曲中存在米酵菌酸残留的现象，为保健食品和中药材中生物毒素的风险监控提供了重要的科技支撑。该方法简单、快速、灵敏度高，适用于六神曲中生物毒素米酵菌酸残留量的测定。

关键词: 超高效液相色谱-串联质谱, 六神曲, 米酵菌酸, 生物毒素

Abstract: A method for the rapid determination of biotoxin (bongkrekic acid) in the Liushenqu was established using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted with methanol by ultrasonication, then the pH was adjusted to 8 using ammonia. After filtration, the extract was purified using an Oasis Max strong anion exchange resin column. The Waters HSS T3 column (100 mm×2.1 mm, 1.8 μm) was used for the UPLC-MS/MS analysis. The mobile phase was acetonitrile-10 mmol/L ammonium formate solution (containing 0.1% (v/v) formic acid). MS analysis was performed using an electrospray ionization (ESI) source in the negative and multiple reaction monitoring (MRM) modes. Under the optimum conditions, the linear range of bongkrekic acid was 0.5-100 μg/L (correlations coefficient (R2)>0.99). The recoveries of the bongkrekic acid were 80.6%-85.3%. The intra-day and inter-day relative standard deviations (RSDs) were in the range of 4.2%-6.8% and 8.2%-13.2%, respectively. The limit of detection (LOD) and limit of quantification (LOQ) were 0.4 μg/kg and 1.2 μg/kg, respectively. The results showed that bongkrekic acid residues were detected in Liushenqu, thereby confirming the supporting role of our method for the risk monitoring of biotoxins in health foods and Chinese herbal medicines. This method is simple, easy, sensitive, and suitable for the determination of the bongkrekic acid residues in Liushenqu.

Key words: biotoxin, bongkrekic acid, Liushenqu, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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