液相色谱-串联质谱法测定白酒中紫杉醇和三尖杉宁碱含量

Simultaneous determination of taxol and cephalomannine in white spirit by liquid chromatography-tandem mass spectrometry

中文关键词:  红豆杉  紫杉醇  三尖杉宁碱  液相色谱-串联质谱法

英文关键词:taxus  taxol  cephalomannine  white spirit  liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry, LC-MS/MS)检测白酒中红豆杉特征组分紫杉醇和三尖杉宁碱含量的方法。方法 样品经甲醇-水(7:3, V/V)提取液提取, 采用水(A)和甲醇(B)作为流动相进行梯度洗脱, 外标法定量, 质谱采用电喷雾电离正模式(positive electrospray ionizationm, ESI+)和多离子检测模式(multiple reactions monitoring, MRM)对紫杉醇和三尖杉宁碱的定量离子、定性离子进行监测。结果 在50~1000 ng/L范围内, 紫杉醇和三尖杉宁碱呈良好的线性关系, 相关系数r2不小于0.995, 方法的检出限为2.5 μg/kg, 定量限为8.3 μg/kg。紫杉醇和三尖杉宁碱在2.5、7.5、25.0 μg/kg 3个水平下加标回收率为96.4%~115.6%, 相对标准偏差不超过2.53%(n=6)。用该方法检测市售红豆杉果实酒、红豆杉树皮酒, 均检测出紫杉醇和三尖杉宁碱。结论 该方法便捷、高效、准确、灵敏, 可用于测定非法添加红豆杉保健酒中紫杉醇和三尖杉宁碱含量。

英文摘要:

      Objective To establish a method for the determination of taxus characteristic components taxol and cephalomannine in white spirit by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Samples were extracted with methanol-water (7:3, V/V) solution. Gradient elution was carried out by usingwater (A) and methanol (B)as mobile phase, and external standard method was used for quantitative analysis.Positive electrospray ionization(ESI+) and multiple reactions monitoring(MRM)mode were used to monitor the quantitative and qualitative ions of paclitaxel and harringtonine. Results The calibration curves showed a good linearity in the range of 50-1000 ng/L and the correlation coefficients r2 were no less than 0.995.The detection limit for the taxol and cephalomannine was 2.5 μg/kg, and the limit of quantitation for the taxol and cephalomannine was 8.3 μg/kg. The recoveries were ranged from 96.4%-115.6% for the taxol and cephalomannine with 3 spiked levels of 2.5, 7.5 and 25.0 μg/kg. and the relative standard deviations (RSDs) were less than 2.53% (n=6). Taxol and cephalomannine were detected in taxus fruit wine and taxus bark wine sold in the market by this method. Conclusion The proposed method is convenient, efficient, accurate and sensitive, which is suitable for detecting taxol and cephalomannine in illegally added taxus health wine.