超高效液相色谱-串联质谱法检测具有治疗镇咳平喘功效的药物成分

Detection of medicinal components with anti-tussive and anti-asthmatic effects by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱-串联质谱法检测镇咳平类药物中4种药物成分的检测方法。方法采用C18色谱柱进行分离,以水(2 mmol/L甲酸铵-50 mmol/L甲酸)-乙腈(2 mmol/L甲酸铵-50 mmol/L甲酸)作为流动相进行梯度洗脱,采用正离子电喷雾,多反应监测模式(multiple reaction monitoring, MRM)进行定性定量测定。结果在线性范围0.05~2μg/g区间内,方法相关性较好,检出限为0.02μg/g,定量限为0.05μg/g。方法回收率为85%~103%,相对标准偏差为1.02%~3.69%。结论方法灵敏度好、精密度高、操作简便,适合应用于此类保健食品中非法添加药物成分的检测。

Objective To establish a method for the determination of four drug components in anti-tussive and anti-asthmatic by ultra performance liquid chromatography tandem mass spectrometry. Methods The C18 chromatographic column was used for separation. Gradient elution was performed using water(2 mmol/L ammonium formate-50 mmol/L formic acid)-acetonitrile(2 mmol/L ammonium formate-50 mmol/L formic acid) as the mobile phase. Positive ion electrospray and multiple reaction monitoring(MRM) were used for qualitative and quantitative determination. Results The correlation was good in the linear range of 0.05-2 μg/g, the limit of detection was 0.02 μg/g, the limit of quantitative was 0.05 μg/g. The recoveries were 85%-103% and the RSDs were 1.02%-3.69%. Conclusion The method has good sensitivity, high precision and simple operation, which is suitable for the detection of illegally added drug components in this kind of health food.