超高效液相色谱-串联质谱法同时检测中药材及植物性食品中23种有毒生物碱

Simultaneous determination of 23 kinds of toxic alkaloids in Chinese medicinal materials and plant-derived food by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  生物碱  超高效液相色谱-串联质谱法  中药材  植物性食品

英文关键词:alkaloids  ultra performance liquid chromatography-tandem mass spectrometry  Chinese medicinal materials  plant-derived foods

中文摘要:

      目的 建立一种超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定中药材及植物性食品样品中23种有毒生物碱的检测方法。方法 样品用氢氧化钠调节pH至7.5, 加入硼砂-氢氧化钠缓冲液, 乙酸乙酯萃取, 氮吹近干后, 用UPLC-MS/MS法同时对23种生物碱进行定性定量分析, 外标法定量。结果 在相应的质量浓度范围内, 23种生物碱在不同基质样品中均有良好的线性关系, 相关系数在0.9989~0.9999。全部样品回收率为61.2%~107.3%, 相对标准偏差为1.1%~8.4%。各类样品检出限为0.01~0.40 μg/kg, 定量限为0.03~1.33 μg/kg。结论 本方法简单、准确、快速, 可实现23种常见生物碱的多组分同时测定, 为生物碱中毒的快速筛查和确证提供了检测时间上的优势, 可用于疑似中药材和植物性食品生物碱中毒的应急事件处理, 并为临床治疗提供技术支撑。

英文摘要:

      Objective To establish a method for the simultaneous determination of 23 kinds of toxic alkaloids in Chinese medicinal materials and plant-derived food by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Firstly, the pH of the samples was adjusted to 7.5 by sodium hydroxide, and then boric acid-sodium hydroxide buffer solution was added, and extracted by ethyl acetate, which followed by concentrated with nitrogen, and detected by UPLC-MS/MS, quantified with external standards. Results The calibration curves of 23 kinds of alkaloids showed good linearities in the corresponding range of mass concentration with correlation coefficients of 0.9989?0.9999. The recoveries of all samples were 61.2%?107.3%, and the RSDs were 1.1%?8.4%, with the limits of detection from 0.01 to 0.40 μg/kg and the limits of quantitation from 0.03 to 1.33 μg/kg. Conclusion This method is rapid, sensitive and accurate, which can realize the simultaneous determination of 23 kinds of common alkaloids, and provides the time advantage of detection for the rapid screening and confirmation of alkaloid poisoning, and the method could be used for emergency treatment of alkaloid poisoning from suspected Chinese medicinal materials and plant-derived foods, and provides technical support for clinical treatment.