普洱茶中HT-2毒素假阳性结果的分析
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摘要
普洱茶叶样品采取有机溶剂(甲醇/水/甲酸70∶29∶1溶液)提取,提取液通过PriboFastRMulti-Toxin IAC免疫亲和净化柱及M226多功能净化柱对比净化,利用超高液相色谱串联质谱的多反应监测模式进行测定分析,采用内标法定量,通过基质加标回收实验、质控已知样实验进行验证.HT-2毒素的回归方程有良好的线性关系,相关系数为0.9995,3个不同加标水平回收率为85.3%—92.6%,相对标准偏差为4.24%—5.61%.174件云南普洱茶叶中,通过免疫亲和柱净化处理的检测结果为未检出,通过多功能净化住净化处理的检测结果有52件确认为假阳性样品,含量范围为0.52—14.27μg·kg~(-1),假阳性率为29.8%.
Samples were extracted by organic solvent(methanol-water-formic acid 70∶29∶1 solution), purified by PriboFast RMulti-Toxin IAC immunoaffinity purification column, determined and analyzed by multi-reaction monitoring of ultra-high performance liquid chromatography tandem mass spectrometry, and quantified by internal standard method, through standard addition recovery experiment, quality control of known samples to verify the comparison. The regression equation of HT-2 toxin has a good linear relationship with a correlation coefficient of 0.9995. The recovery rates at three different levels are 85.3% — 92.6%, and the relative standard deviations are 4.24% —5.61%. Among the 174 Yunnan Pu-erh teas, the detection results by the immunoaffinity column purification treatment were not detected, and 52 samples were confirmed as false positive samples by the multi-function purification and purification treatment, with a false positive rate of 29.8%, with the content ranged of 0.52—14.27 μg·kg~(-1).
Samples were extracted by organic solvent(methanol-water-formic acid 70∶29∶1 solution), purified by PriboFast RMulti-Toxin IAC immunoaffinity purification column, determined and analyzed by multi-reaction monitoring of ultra-high performance liquid chromatography tandem mass spectrometry, and quantified by internal standard method, through standard addition recovery experiment, quality control of known samples to verify the comparison. The regression equation of HT-2 toxin has a good linear relationship with a correlation coefficient of 0.9995. The recovery rates at three different levels are 85.3% — 92.6%, and the relative standard deviations are 4.24% —5.61%. Among the 174 Yunnan Pu-erh teas, the detection results by the immunoaffinity column purification treatment were not detected, and 52 samples were confirmed as false positive samples by the multi-function purification and purification treatment, with a false positive rate of 29.8%, with the content ranged of 0.52—14.27 μg·kg~(-1).
引文