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

作　　者：黄媛 王晓阳 于佳 谷岩 程亮 李志远 孔祥翔 HUANG Yuan;WANG Xiao-Yang;YU Jia;GU Yan;CHENG Liang;LI Zhi-Yuan;KONG Xiang-Xiang(Liaoning Inspection,Examination&Certification Centre,Shenyang 110000,China;Shenyang Yupu Technology Co.,Ltd.,Shenyang 110000,China;Shanghai AB Sciex Analytical Instrument Trading Co.,Ltd.,Beijing 100015,China;Liaoning Provincial Institute for Drug Inspection and Testing,Shenyang 110000,China)

机构地区：[1]辽宁省检验检测认证中心,沈阳110000 [2]沈阳誉普科技有限公司,沈阳110000 [3]上海爱博才思分析仪器贸易有限公司,北京100015 [4]辽宁省药品检验检测院,沈阳110000

出　　处：《食品安全质量检测学报》2025年第6期216-223,共8页Journal of Food Safety and Quality

基　　金：基于三重四极杆串联质谱仪联合Q-TRAP方法建立食品中违法添加植物类泻药成分的筛查平台项目(2023-MS-065)。

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0.25~5.00μg/m L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0.05~1.00μg/m L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。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 0.25–5.00μg/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 0.05–1.00μg/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.

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 减肥食品 筛查 定量 

分 类 号：O657.63[理学—分析化学] TS207.3[理学—化学]