色谱

色谱

• 研究论文 • 上一篇    下一篇

免疫亲和柱净化-液相色谱-串联质谱法测定中药材中的14种真菌毒素

葛宝坤*, 赵孔祥, 王伟, 宓捷波   

  1. 天津出入境检验检疫局, 天津 300461
  • 收稿日期:2011-01-20 修回日期:2011-02-25 出版日期:2011-06-28 发布日期:2011-07-25
  • 通讯作者: 葛宝坤,研究员,主要研究食品中农兽药残留、生物毒素及添加剂检测. Tel: (022)66273154
  • 基金资助:

    国家质量监督检验检疫总局科研课题资助项目(2008IK144).

Determination of 14 mycotoxins in Chinese herbs by liquid chromatography-tandem mass spectrometry with immunoaffinity purification

2, 2, 2   

  1. Tianjin Entry & Exit Inspection and Quarantine Bureau, Tianjin 300461, China
  • Received:2011-01-20 Revised:2011-02-25 Online:2011-06-28 Published:2011-07-25

PDF

713

被引次数

48

摘要： 依次采用磷酸盐缓冲液(PBS)和甲醇-PBS溶液提取样品,以多功能免疫亲和柱净化,采用液相色谱-串联四极杆质谱检测,可同时测定中药材中的黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、伏马毒素B1、伏马毒素B2、T-2毒素、HT-2毒素、赭曲霉毒素A(OTA)、玉米赤霉烯酮等14种真菌毒素。优化条件下,真菌毒素的定量限(LOQ)为1～5 μg/kg, 4种中药材基质(人参、桔梗、板蓝根、麦门冬)中3个不同添加水平的平均回收率(n=6)为71.9%～99.7%,相对标准偏差(RSD)为4.8%～15.8%。该方法的检测速度快,中药材复杂基质的干扰较少,结果准确、可靠,定量限可满足国内外中药材真菌毒素相关限量的要求。

关键词: 免疫亲和柱净化, 液相色谱-串联质谱, 真菌毒素, 中药材

Abstract: A method was developed for the determination of 14 mycotoxins, aflatoxins, T-2, HT-2, fumonisins, ochratoxin A, zearalenone, etc. in Chinese herbs by liquid chromatography-tandem quadrupole mass spectrometry (LC-MS/MS). The sample was extracted with phosphate buffer solution (PBS) and methanol in turn, and then purified by a high selective multifunctional immunoaffinity column. The column was washed by PBS (containing 0.1% Twain) and water, and then eluted by methanol. The eluate was dried under nitrogen, dissolved in methanol-10 mmol/L NH4Ac （40:60, v/v） solution. The mycotoxins were separated on a Waters Xterra C18 MS column (100 mm×2.1 mm, 3.5 μm) and detected by MS/MS. The limits of quantification (LOQs) of the 14 mycotoxins were from 1.0 to 5.0 μg/kg. The average recoveries of the 14 mycotoxins spiked in Chinese herbs (Ginseng, Campanulaceae, Radix and Ophiopogonis) ranged from 71.9% to 99.7% at the three spiked levels of 1.0, 5.0, 10.0 μg/kg, and the relative standard deviations (RSDs, n=6) were between 4.8% and 15.8%. The method is rapid, sensitive and accurate, and suitable for the determination of the 14 mycotoxins in Chinese medicines. The quantification limits of aflatoxins can meet the domestic and foreign requirements.

Key words: Chinese herbs, mycotoxins, immunoaffinity column purification, liquid chromatography-tandem mass spectrometry (LC-MS/MS)