UPLC-QTRAP同时检测8种新型策划药

目的建立一种简单、快速的超高压液相色谱-串联质谱(UPLC-MS/MS)联用法同时检测毛发样品中8种新型策划药。方法毛发样品经冷冻研磨超声后,通过Phenomenex Kinetex~?F5 100á(50mm×2.1mm,2.6μm)色谱柱进行分离,以5 mmol/L乙酸铵和甲醇为流动相,0.35mL/min流速进行梯度洗脱。在电喷雾离子源正离子(ESI+)模式下,质谱采集使用独有的多反应监测-信息依赖式采集-增强子离子扫描(MRM-IDA-EPI)模式。结果 8种新型策划药在0.1-100 ng/mL的浓度范围内线性关系良好(r≥0.9999)。检出限为1.5 ng/g,5 ng/g、50 ng/g、2500ng/g 3个添加水平的回收率在92.46%~105.70%之间。日间精密度RSD在0.39%~7.67%之间、日内精密度的RSD在0.37%~7.54%之间(n=9)。结论本方法简单快速、特异性强,可同时对毛发样品中8种新型策划药进行定性定量分析。

Simultaneously detectmination of eight new designer drugs in hair by UPLC-QTRAP

Objective A simple and rapid method was established for simultaneous detection of 8 new designer drugs in hair by ultra high liquid chromatography-tandem quadrupole complex linear ion trap mass spectrometry(UPLC-MS/MS). Methods The hair samples were processed by a frozen grinding ultrasonic machine, separated by chromatographic column(Phenomenex Kinetex~? F5 100á 50 mm×2.1 mm, 2.6μm). Gradient elution was performed with 5 mmol/L ammonium acetate and methanol as mobile phases at a flow rate of 0.35 mL/min. In the electrospray ion source positive ion mode(ESI+), the mass spectrometry was performed in the unique multi-response monitoring-information-dependent acquisition-enhancer ion scanning(MRM-IDA-EPI) mode. Results The linearity of 8 new designer drugs was good in the concentration range of 0.1-100 ng/mL(r ≥ 0.9999). The LOD was 1.5 ng/g, and the recoveries of 5, 50 and 2500 ng/g were between 92.46%~105.70%. The inter-day precision(RSD) ranged from 0.39%~7.67%, and the intraday precision(RSD) ranged from 0.37%~7.54%(n=9). Conclusion This method is simple, rapid and specific, and can be used for qualitative and quantitative analysis of the 8 new designer drugs in hair.