Simultaneous Determination of Eight Tranquilizers in Pork by Ultra-Performance Liquid Chromatography Coupled with Electrospray Tandem Mass Spectrometry

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• 作者：Liqun Zhang ; Pinggu Wu ; Quan Jin ; Haipeng Ye ; Xihui Huang…
• 关键词：Tranquilizers ; Solid phase extraction ; Matrix effect ; LC ; MS ; MS
• 刊名：Food Analytical Methods
• 出版年：2017
• 出版时间：February 2017
• 年：2017
• 卷：10
• 期：2
• 页码：354-362
• 全文大小：
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Food Science; Chemistry/Food Science, general; Microbiology; Analytical Chemistry;
• 出版者：Springer US
• ISSN：1936-976X
• 卷排序：10

文摘

An ultra-performance liquid chromatography/electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) method was developed and validated for quantification of eight tranquillizers (chlorpromazine, imipramine hydrochloride, diazepam, nitrazepam, nordazepam, oxazepam, flurazepam, and haloperidol) in pork. Sample pretreatment consisted of extraction by acetonitrile, defatted by n-hexane, and further solid phase extraction by hydrophilic-lipophilic balance (HLB) extraction cartridges. The triple quadrupole mass spectrometer was operated in positive ion mode, and multiple reaction monitoring was used for drug quantification. The method was validated over the concentration ranges of 1.0 ∼ 250 μg kg−1 for the eight tranquillizers. The calibrations were performed in sample matrices, and the interference effect of sample matrices on the ionization was effectively eliminated. Good linear relationship (R2 > 0.99) was observed within the concentration range of 1.0–250 μg kg−1. The average recoveries of the eight tranquillizers spiked at three levels ranged from 63.7 to103.2 % with the relative standard deviation below 11.8 %. The limits of detection were between 0.06 and 0.30 μg kg−1, and the limits of quantification were between 0.2 and1.0 μg kg−1 for all analytes in pork. This validated method has been successfully used to quantify the concentration of the eight tranquillizers in pork samples.