液相色谱-四级杆-静电轨道阱高分辨质谱法测定保健食品中降压类药物

Determination of antihypotensive drugs in health food by liquid chromatography-quadrupole-orbitrap high resolution mass spectrometry

目的建立一种液相色谱-四级杆-高分辨质谱仪测定保健食品中11种降压类药物的分析方法。方法采用甲醇-水混合溶液超声提取,滤膜过滤,采用0.1%甲酸和乙腈作为流动相进行梯度洗脱,质谱(ESI+)采用全扫描(fullscan)+数据依赖MS2(ddMS2)检测模式对降压类药物进行监测,根据母离子及子离子精确质量数进行定性与定量分析。结果11种降压药分离完全,线性范围均为2.0~100μg/L,相关系数(r2)均不低于0.9915,平均回收率为72.4%~97.1%,相对标准偏差为5.0%~13.9%,液体类样品定量限为0.5~2.5μg/kg,固体类样品定量限为2.5~12.5μg/kg。结论该方法快速、灵敏,适合测定保健食品中降压类药物。

Objective To establish a method for determination of 11 kinds of antihypertensive drugs in health food by liquid chromatography-quadrupole-orbitrap high resolution mass spectrometry (LC-Q-Orbitrap). Methods The antihypertensive drugs in samples were extracted by ultrasound extraction with methanol-water mixed solvent, and determined after filtration with membrane. The drugs were separated on a reversed phase column using a gradient elution program of 0.1% formic acid aqueous solution and acetonitrile. The LC-Q-Orbitrap (ESI+) with fullscan and data dependency MS2(ddMS2) was used, and identification of the 11 kinds of antihypertensive drugs was performed based upon the exact mass of mother ion and product ion. Results The 11 kinds of antihypertensive drugs were completely separated with a linear range of 2.0 to 100 μg/L. The correlation coefficients (r 2 ) were not less than 0.9915. The average recoveries were from 72.4% to 97.1% and the relative standard deviations were from 5.0% to 13.9%. The limits of quantitation (LOQs) of liquid samples were from 0.5 to 2.5 μg/kg, and those of solid samples were from 2.5 to 12.5 μg/kg. Conclusion This method is rapid and sensitive, which is suitable for determination of antihypertensive drugs in health food.