超高效液相色谱-串联质谱法测定普洱茶中赭曲霉毒素A

Determination of ochratoxin A in Pu-erh tea by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  赭曲霉毒素A  普洱茶  超高效液相色谱-串联质谱法

英文关键词:ochratoxin A  Pu-erh tea  ultra performance liquid chromatography- tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱测定普洱茶中赭曲霉毒素A的分析方法。方法 普洱茶样品采用乙腈:水(7:3,V:V)提取, PriboFast? Multi-Toxin IAC免疫亲和净化柱净化, 超高效液相色谱串联质谱进行测定分析, 采用内标法定量。结果 赭曲霉毒素A在浓度0.5~199.5 μg/L范围内具有良好的线性关系, 相关系数为0.9993, 3个加标水平下的回收率为92.5%~95.6%, 相对标准偏差为2.18%~3.25%, 检出限为0.1 μg/kg。普洱茶样品中的赭曲霉毒素A均为未检出。结论 普洱茶中复杂基质的存在对赭曲霉毒素A的测定有干扰, 应采用免疫亲和净化柱净化处理, 该方法具有较高的灵敏度及准确度, 适用于普洱茶中赭曲霉毒素A的实际检测。

英文摘要:

      Objective To establish a method for the determination of ochratoxin A in Pu-erh tea by high performance liquid chromatography-tandem mass spectrometry. Methods Pu-erh tea samples were extracted with acetonitrile/water (7:3, V:V), purified by PriboFast? Multi-Toxin IAC immunoaffinity purification column, and analyzed by ultra performance liquid chromatography tandem mass spectrometry, and quantified by internal standard method. Results Ochratoxin A had a good linear relationship in the concentration range of 0.5?199.5 μg/L, the correlation coefficient was 0.9993, the recovery rates at the 3 spiked levels were 92.5%?95.6%, the relative standard deviations were 2.18%?3.25%, and the limit of detection was 0.10 μg/kg. Ochratoxin A in Pu-erh tea samples was not detected. Conclusion The presence of a complex matrix in Pu-erh tea interferes with the determination of ochratoxin A. The sample should be purified using an immunoaffinity purification column. This method has high sensitivity and high accuracy, which is suitable for the actual detection of ochratoxin A in Pu-erh tea.