高效液相色谱-串联质谱法定性定量测定鱼腥草中马兜铃酸类物质

Qualitative and quantitative determination of aristolochic acids in Houttuynia cordata by high performance liquid chromatography- tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  马兜铃酸类物质  鱼腥草

英文关键词:high performance liquid chromatography-tandem mass spectrometry  aristolochic acids  Houttuynia cordata

中文摘要:

      目的 建立高效液相色谱-三重四极杆质谱法快速检测鱼腥草中9种马兜铃酸类物质的分析方法。 方法 采用A CQUITY UPLC? HSS T3色谱柱(100 mm×2.1 mm, 1.8 μm), 0.1%甲酸-5 mmol/L-水溶液(A)及甲醇(B)为流动相, 梯度洗脱, 流速为0.35 mL/min, 柱温为40 ℃, 采用正离子多反应监测模式进行检测。结果 9种马兜铃酸类物质在线限范围内线性关系良好(r>0.9990), 平均加样回收率(n=6)为89.62%~107.61%, 相对标准差≤5.18%。此批鱼腥草样品中马兜铃酸(A、B、C、D)、7-羟基马兜铃酸A、马兜铃内酰胺、马兜铃酮均未检出, 马兜铃内酰胺F1含量最低值为0.376 mg/kg, 含量最高值为7.034 mg/kg; 马兜铃内酰胺BII含量最低值为0.984 mg/kg, 含量最高值为11.931 mg/kg。结论 此方法灵敏度高、可重复性好、回收率较高、操作简便、效率高, 适用于鱼腥草中多种马兜铃酸类化合物的检测。

英文摘要:

      Objective To establish a method for the determination of 9 kinds of ristolochic acids in Houttuynia cordata by high performance liquid chromatography-triple quadrupole mass spectrometry. Methods A CQUITY UPLC? HSS T3 column (100 mm×2.1 mm, 1.8 μm) was used, 0.1% formic acid-5 mmol/L-aqueous solution (A) and methanol (B) were used as mobile phases, gradient elution was carried out, the flow rate was 0.35 mL/min, the column temperature was 40 ℃, and the positive ion multi-reaction monitoring mode was used for detection. Results The linear range of 9 aristolochic acids was good (r>0.9990), and the average recoveries (n=6) were 89.61%-107.61%, relative standard deviation≤5.18%. Aristolochic acid (A, B, C, D), 7-hydroxyaristolochic acid A, aristolochic lactam and aristolochic ketone in this batch of Houttuynia cordata samples were not detected. The lowest content of aristolochic lactam F1 was 0.376 mg/kg, and the highest content was 7.034 mg/kg. The lowest content of aristolochia lactam BII was 0.984 mg/kg, and the highest content was 11.931 mg/kg. Conclusion This method has high sensitivity, good repeatability, high recovery rate, simple operation and high efficiency, which is suitable for the detection of various aristolochic acids in Houttuynia cordata samples.