Rapid screening of 10 drugs in blood using ultra performance liquid chromatography with high resolution quadrupole-time-of-flight mass spectrometry

doi:10.3724/SP.J.1123.2016.01028

Abstract

Abstract:

A high-throughput method was developed for rapid screening of 10 drugs in blood by ultra performance liquid chromatography with high resolution quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF/MS). The sample was extracted by ethyl acetate, the extraction solution was concentrated to near dryness, and dissolved with methanol. Then the sample was passed through a 0.22 μ m membrane. The separation of the 10 target compounds was performed on a Waters ACQUITY UPLC@BEH C18 column (100 mm×2.1 mm, 1.7 μ m) with gradient elution using methanol and 0.1% (v/v) formic acid aqueous solution as mobile phases, and analyzed by UPLC-Q-TOF/MS under electrospray ionization (ESI) mode with scanning range of m/z 50-1000. Rapid screening can be achieved using MS matching scores, deviation of retention time, measured mass, isotopic abundance matching scores, isotope spacing match scores and MS/MS matching scores. Good linearities were observed in the range of 10.0-500.0 μ g/L with the correlation coefficients from 0.9908 to 0.9958. The limits of detection and the limits of quantification were 1.0-2.0 μ g/L and 4.0-8.0 μ g/L, respectively. The spiked recoveries were 56.7%-83.0% with the relative standard deviations of 3.6%-8.9%. The result screening database was built using Agilent Mass Hunter PCDL Manager software and then used for the analysis of spiked samples. MS matching scores, isotopic abundance matching scores, isotope spacing matching scores (all > 90 points) and MS/MS matching scores (> 70 points) were applied to identify the drugs. The results showed that all the spiked drugs could be correctly identified with low deviations of retention time (< 0.1 min) and mass (< 1 mDa). The developed method is suitable for the screening and confirmation of the drugs in forensic and clinical analytical toxicology.

Key words: blood, drugs, quadrupole-time-of-flight mass spectrometry (Q-TOF/MS), rapid screening, ultra performance liquid chromatography (UPLC)

CLC Number:

O658

SHI Yintao, WANG Huijun, GUO Jingqi, DING Jing, WANG Junwei. Rapid screening of 10 drugs in blood using ultra performance liquid chromatography with high resolution quadrupole-time-of-flight mass spectrometry[J]. Chinese Journal of Chromatography, 2016, 34(5): 538-542.

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