超高效液相色谱-串联质谱法同时测定蜂蜜中雷公藤和乌头类10种植物毒素

Simultaneous determination of 10 kinds of phytotoxins of tripterygium wilfordii and aconitum in honey by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  植物毒素  雷公藤类毒素  乌头类毒素  蜂蜜  超高效液相色谱串联质谱

英文关键词:phytotoxin  tripterygium wilfordii toxoid  aconitum toxoid  honey  ultra performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-串联质谱法同时测定蜂蜜中雷公藤类、乌头类10种植物毒素的方法。方法 样品采用1%甲酸水-70%乙腈水溶液涡旋提取, 经高速离心后, 取上清液加入适量N-丙基乙二胺(primary secondary amine, PSA), 振荡混匀, 过0.22 μm滤膜, 上机测定分析, 采取基质工作曲线, 外标法定量。结果 10种植物毒素的检出限为0.03~1.90 μg/kg。10种植物毒素在一定的质量浓度范围内线性关系良好, 相关系数均大于0.999。3种不同浓度加标水平下, 植物毒素的平均加标回收率范围为89.5%~113.8%, 相对标准偏差为0.5%~8.7%。结论 该测定方法操作便捷、灵敏度高, 准确性强, 为应急事件中植物毒素快速筛查提供技术支持, 适用于实验室对蜂蜜样品特别是批量样品中多种植物毒素的同时测定分析。

英文摘要:

      Objective To establish a method for the simultaneous determination of 10 kinds of phytotoxins, including tripterygium wilfordii and aconite in honey by ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted by vortexing with 1% formic acid water-70% acetonitrile water solution. After high-speed centrifuged, added appropriate amount of primary secondary amine (PSA) to the supernatant, and shaked and mixed evenly, passed through 0.22 μm filter membrane, then determined and analyzed by the instrument. The matrix working curve was used for quantification by the external standard method. Results The limits of detection of 10 kinds of phytotoxins were 0.03–1.90 μg/kg. The 10 kinds of phytotoxins showed good linearity in a certain range of mass concentration with the correlation coefficients were all greater than 0.999. The average recovery rates of toxins ranged from 89.5% to 113.8% at 3 kinds of different concentration spiked levels, and the relative standard deviations of 0.5%–8.7%. Conclusion The method is convenient, sensitive and accurate, and provides technical support for rapid screening of phytotoxins in emergencies.?It is suitable for simultaneous determination of various phytotoxins in honey samples, especially in batch samples.