超高效液相色谱串联四级杆飞行时间质谱法检测毒蘑菇中4种常见毒素含量

Determination of 4 kinds of common toxins in poisonous mushrooms by ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry

中文关键词:  超高效液相色谱串联四级杆-飞行时间串联质谱法  毒蝇碱  毒蝇母  鹅膏蕈氨酸  脱磷酸裸盖菇素

英文关键词:ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry  muscarine  muscimol  ibotenic acid  psilocin

中文摘要:

      目的 建立超高效液相色谱串联四级杆飞行时间质谱法快速检测毒蘑菇中毒蝇碱、毒蝇母、鹅膏蕈氨酸、脱磷酸裸盖菇素4种强毒性毒素含量的分析方法。方法 新鲜蘑菇样品经过一系列的前处理后, 待测样品经ACQUITY UPLC BEH Amide色谱柱(100 mm×2.1 mm, 1.7 μm)分离, 以甲醇-5 mmol/L乙酸铵水(20:80, V:V)为流动相进行梯度洗脱, 流速为0.3 mL/min, 柱温为26 ℃, 外标法定量检测。结果 在一定浓度范围内, 4种毒素的线性关系良好, 相关系数大于0.999, 3水平加标回收率为86.7%~110.6%, 相对标准偏差为3.5%~6.2%, 检出限为0.0002~5.0 μg/mL。结论 该方法灵敏、准确、特异性好, 适用于蘑菇中毒蝇碱、毒蝇母、鹅膏蕈氨酸、脱磷酸裸盖菇素的检测。

英文摘要:

      Objective To establish a method for rapid determination of 4 common toxins including musearine, muscimol, ibotenic acid, psilocin in poisonous mushrooms by ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry. Methods After a series of pre-treatments of fresh mushroom samples, the tested samples were separated with an ACQUITY UPLC BEH Amide column (100 mm×2.1 mm, 1.7 μm) at the flow rate of 0.3 mL/min by gradient elution using methanol-5 mmol/L ammonium acetate water (20:80, V:V) as mobile phase. The temperature of the column was maintained at 26 ℃, and the content was quantitatively analyzed by external standard method. Results The linear relationship of the 4 toxins was good within a certain concentration range, and the correlation coefficients were greater than 0.999. The recoveries of 3 levels were 86.7%?110.6%, the relative standard deviations were 3.5%?6.2%, and the limits of detection were 0.0002?5.0 μg/mL. Conclusion This method is sensitive, accurate and specific, and is suitable for the detection of mushroom musearine, muscimol, ibotenic acid and psilocin.