UPLC-Q-TOF/MS快速测定保健食品中32种毒品及处方药物

Rapid determination of 32 drugs in dietary supplements by ultra-high performance liquid chromatography-quadrupole-time-of-fight mass spectrometry

目的建立一种超高效液相色谱-四极杆-飞行时间质谱(HPLC-Q-TOF/MS)快速测定保健食品中32种毒品及处方药物的方法。方法样品经甲醇超声提取,经飞诺美Luna Omega C18(2.1×100 mm,1.6μm)色谱柱分离,以0.1%甲酸水溶液-乙腈为流动相梯度洗脱,HPLC-Q-TOF/MS检测。结果利用32种化合物的母离子精确质量数,保留时间,同位素丰度比和二级碎片信息构建标准谱库,实现对可疑样品中目标物的定性筛查。方法学考察显示,32种化合物在各自线性范围内线性关系良好,相关系数r;>0.993,在一般固体、液体、高蛋白、高脂肪样品中方法检出限范围10~20μg/kg,方法定量限均为50μg/kg,平均回收率为83.63%~116.91%,相对标准偏差(RSD)为0.62%~10.85%。结论该方法用于保健食品中毒品及处方药物分析,具有前处理简单、检测速度快、适用范围广、对标品依赖性低的特点,适合司法鉴定技术人员在日常案件侦办中使用。

Objective To establish an analytical method for the determination of 32 drugs in dietary supplements by ultra-high performance liquid chromatography-quadrupole-time-of-fight mass spectrometry.Methods The samples were processed by ultrasonic extraction with methanol,and separated by Phenomenex Luna Omega C18(2.1×100 mm,1.6μm)column,followed by gradient elution with 0.1%formic acid and acetonitrile as the mobile phase.Results An illegal additive library for 32 chemicals was established by accurate mass,retention time,isotopic ratio and MS/MS spectrum.It can be used for qualitative detection of the target compounds in suspect samples.The validation results indicated that all the 32 chemicals had good linear relationships with correlation coefficients(r;)greater than 0.993.In the general solid,liquid,high protein,high fat matrixes,the limits of detection(LOD)for the 32 chemicals were in the range of 10~20μg/kg,while the limits of quantitation(LOQ)were 50μg/kg.The average recoveries of the 32 chemicals ranged from 83.63%to 116.91%with relative standard deviations(RSD)from 0.62%to 10.85%.Conclusion This method has the advantages of simple pretreatment,fast detection speed,wide application range and low dependence on standard products,and can be applied for the determination of drugs and prescription drugs in health food.It is suitable for judicial authenticators to use in daily case investigation.