高效液相色谱-串联质谱法测定降压类保健食品中5种α-受体阻断剂类非法添加药物的含量

Simultaneous determination of 5 kinds of α-receptor antagonists in antihypertensive health foods by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  α-受体阻断剂  非法添加  保健食品

英文关键词:high performance liquid chromatography-tandem mass spectrometry  α-receptor antagonists  illegally added chemical  health foods

中文摘要:

      目的 建立高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)法检测降压类保健食品中5种α-受体阻断剂含量的检测方法。方法 样品经甲醇提取, 残留物经Waters Sunfire C18 (100 mm×2.1 mm, 5 μm)色谱柱分离, 以0.1%甲酸水溶液-0.1%甲酸乙腈溶液为流动相梯度洗脱, 流速为0.3 mL/min, 采用多反应监测正离子模式, 定性和定量测定降压类保健食品中酚妥拉明、妥拉唑林、哌唑嗪、特拉唑嗪和育亨宾等5种α-受体阻断剂。结果 5种α-受体阻断剂分别在0.5~160 μg/L浓度范围内呈现良好的线性关系, 相关系数均大于0.993; 酚妥拉明和哌唑嗪方法的检出限为5 μg/kg, 定量限为10 μg/kg; 特拉唑嗪和育亨宾的检出限为2 μg/kg, 定量限为5 μg/kg; 妥拉唑林的检出限为15 μg/kg, 定量限为40 μg/kg; 添加水平分别为10~100、5~50、40~400 μg/kg时, 样品平均回收率为81.6%~113.5%, 相对标准偏差为0.69%~4.80% (n=5)。结论 该方法简便、快捷、准确、灵敏度高, 适用于降压类保健食品中非法添加的酚妥拉明、妥拉唑林、哌唑嗪、特拉唑嗪及育亨宾等5种α-受体阻断剂的快速检测。

英文摘要:

      Objective To establish a method for determination of 5 kinds of α-receptor antagonists residues in antihypertensive health foods by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The sample was extracted with methanol, and the residue was separated on a Waters Sunfire C18 (100 mm ×2.1 mm, 5 μm) column. The gradient was eluted with 0.1% aqueous formic acid-0.1% formic acid in acetonitrile as a mobile phase gradient at a flow rate of 0.3 mL/min. Five kinds of α-receptor antagonists such as phentolamine, tolazoline, prazosin, terazosin and yohimbine in antihypertensive health foods were qualitatively and quantitatively determined with positive ion mode with multiple reactions. Results The 5 α-receptor antagonists showed good linear relationships in the range of 0.5-160 μg/L, and the correlation coefficients were greater than 0.993. The detection limits of phentolamine and prazosin were 5 μg/kg, and the limits of quantification were 10 μg/kg. The detection limits of terazosin and yohimbine were 2 μg/kg, and the limits of quantification were 5 μg/kg. The detection limit of tolazoline was 15 μg/kg, and the limit of quantification was 40 μg/kg. When the addition levels were 10-100, 5-50, and 40-400 μg/kg, the average recoveries of samples were 81.6%-113.5%, and the relative standard deviations were 0.69%-4.80% (n=5). Conclusion The method is simple, rapid, accurate and sensitive, which is suitable for rapid detection of 5 kinds of α-receptor antagonists such as phentolamine, tolazoline, prazosin, terazosin and yohimbine illegally added in antihypertensive health food.