超高效液相色谱-四极杆串联离子肼复合质谱法筛查和定量检测减肥食品中8种蒽醌苷元

Screening and quantitative detection of 8 kinds of anthraquinone aglycones in weight-loss foods by ultra performance liquid chromatography-quadrupole ion trap tandem mass spectrometry

中文关键词:  超高效液相色谱-四极杆串联离子肼复合质谱法  蒽醌苷元  番泻苷元A  番泻苷元B  减肥食品  筛查  定量

英文关键词:ultra performance liquid chromatography-Q-trap-tandem mass spectrometry  anthraquinone aglycones  weight-loss foods  screening  quantification

中文摘要:

      目的 建立一种减肥食品中违法添加含蒽醌类植物泻药的筛查和定量方法。方法 采用酸水解提取的方法将食品中蒽醌苷类物质水解为蒽醌苷元, 并用超高效液相色谱-四极杆串联离子肼复合质谱法(ultra performance liquid chromatography-Q-trap-tandem mass spectrometry, UPLC-Q-trap-MS)对水解产生的8种蒽醌苷元进行测定。以多反应监测(multiple reaction monitoring, MRM)作为探针检测, 并通过信息依赖性采集(information dependent acquisition, IDA)触发增强型子离子扫描(enhanced product ion scan, EPI)模式, 采用外标法定量。结果 减肥食品中大黄素甲醚的检出限为5.0 mg/kg, 定量限为12.5 mg/kg, 在0.25~5.00 μg/mL范围内线性关系良好, 其他7种蒽醌苷元的检出限为1.0 mg/kg, 定量限为2.5 mg/kg, 并且在0.05~1.00 μg/mL范围内线性关系良好, 相关系数r≥0.992。分别在2.5、5.0和20.0 mg/kg(大黄素甲醚在12.5、25.0、100.0 mg/kg) 3个浓度水平进行加标回收试验, 8种蒽醌苷元的平均回收率为80.6%~102.0%, 相对标准偏差(relative standard deviations, RSDs)为2.35%~8.80% (n=6)。结论 该方法具有操作简单、灵敏度高、准确度高的特点, 适合于8种蒽醌苷元的同时快速筛查与准确定量。

英文摘要:

      Objective To establish a screening and quantitative method for illegally added anthraquinone- containing plant laxatives in weight-loss foods. Methods The anthraquinone glycosides in foods were hydrolyzed into anthraquinone aglycones by the acid hydrolysis extraction method, and 8 kinds of anthraquinone aglycones produced by hydrolysis were determined by ultra performance liquid chromatography-Q-trap-tandem mass spectrometry (UPLC-Q-trap-MS). Multiple reaction monitoring (MRM) was used as a probe for detection, and the enhanced product ion scan (EPI) mode was triggered through information dependent acquisition (IDA). External standard method was adopted for quantification. Results The limit of detection of physcion in weight-loss foods was 5.0 mg/kg, and the limit of quantification was 12.5 mg/kg, with a good linear relationship in the range of 0.25–5.00 μg/mL. The limits of detection of the other 7 kinds of anthraquinone aglycones were 1.0 mg/kg, and the limits of quantification were 2.5 mg/kg, and they had good linear relationships in the range of 0.05–1.00 μg/mL, with correlation coefficients r≥0.992. Spike recovery tests were carried out at three concentration levels of 2.5, 5.0 and 20.0 mg/kg (physcion at 12.5, 25.0 and 100.0 mg/kg), respectively. The average recovery rates of the 8 kinds of anthraquinone aglycones were 80.6%–102.0%, and the relative standard deviations (RSDs) were 2.35%–8.80% (n=6). Conclusion This method has the characteristics of simple operation, high sensitivity and high accuracy, and is suitable for the simultaneous rapid screening and accurate quantification of 8 kinds of anthraquinone aglycones.