QuEChERS-超高效液相色谱-质谱联用法检测蜂蜜中雷公藤甲素和雷公藤红素及其热稳定性研究

Determination of triptolide and celastrol in honey by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry and research on their thermostability

中文关键词:  蜂蜜  雷公藤甲素  雷公藤红素  超高效液相色谱-质谱联用法  热稳定性

英文关键词:honey  triptolide  celastrol  ultra performance liquid chromatography-tandem mass spectrometry  thermostability

中文摘要:

      目的 建立QuEChERS-超高效液相色谱-串联质谱联用法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定蜂蜜中雷公藤甲素和雷公藤红素的检测方法, 并考察这2种物质在储存和冲泡过程中的热稳定性。方法 样品采用水溶解, 乙腈提取, 氯化钠和无水硫酸镁盐析脱水, N-丙基乙二胺、C18净化粉和磁性纳米粒子分散净化, 超高效液相色谱-串联质谱法进行分析。结果 雷公藤甲素和雷公藤红素定量限分别为0.5和0.16 μg/kg, 在0.5~100 ng/mL浓度范围内线性关系均良好, 加标回收率分别在83.03%~93.33%和82.62%~87.83%范围内。两种物质的含量在冷藏条件下较稳定; 长期贮存时, 其含量随温度升高会产生不同程度的降低。使用80 ℃以上水温冲泡蜂蜜, 2种物质含量有部分下降, 且高温保持3 h后会有显著降低的趋势。雷公藤甲素热稳定性略好于雷公藤红素。结论 该方法快速、灵敏, 适用于蜂蜜中雷公藤甲素和雷公藤红素的批量筛查和痕量分析。2种物质在低温条件下热稳定性较好, 但随着储存或冲泡温度的升高及时间的延长，含量有部分下降。该特征对于蜂蜜中两种毒素的处理具有实际意义。

英文摘要:

      Objective To establish a method for the determination of triptolide and celastrol in honey by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry, and to investigate thermostability of 2 kinds of compounds during storage and dilution process. Methods Sample was dissolved by water and extracted by acetonitrile, following salting out and dehydration with sodium chloride and anhydrous magnesium sulfate, then purified by disperse primary secondary amine, carbon 18 and magnetic nanoparticles, finally analysed by ultra performance liquid chromatography-tandem mass spectrometry. Results Limits of quantitation of triptolide and celastrol were 0.5 and 0.16 μg/kg, the linear relationship was good in the range of 0.5?100 ng/mL, and the recoveries were 83.03%?93.33% and 82.62%?87.83%, respectively. Two kinds of compounds were stable in refrigeration storage, but the content had more or less decreased with storage temperature rising for long period. Partial reduction of two kinds of substances occurred while diluted by water with temperature more than 80 ℃, and there was significantly decreasing trend by kept with that temperature for 3 h. Triptolide had better thermostability than celastrol. Conclusion This method is rapid and sensitive, which is suited for screening and determination of triptolide and celastrol in honey. They have good thermostability at low temperature conditions, but would decrease with higher storage and dilution temperature, and longer time. This character has practical significance.