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建立了血液中佐匹克隆的自动固相萃取-液相色谱-飞行时间质谱(ASPE-LC-Q-TOF/MS)的定性与确证方法。样品经HLB固相萃取柱提取后,在Eclips Plus C18反相柱上分离,外标法定量。方法对佐匹克隆的检出限为0.3μg/L,佐匹克隆质量浓度在1~500μg/L范围内线性良好(R2=0.9993),血液中佐匹克隆的回收率在70%以上,日内、日间RSD不高于7.7%。利用Agilent MassHunter PCDL Manager软件建立佐匹克隆的数据库,并对加标样品进行筛查分析,样品中添加的佐匹克隆保留时间偏差0.002 min,质量偏差0.05 mDa,同位素峰形匹配得分大于98,同位素间距得分大于99,MS/MS图谱匹配得分大于94。方法可用于法庭与临床的毒物分析。
A method for qualitative and confirmatory determination of zopiclone in blood by automatic solid-phase extraction-liquid chromatography-time of flight mass spectrometry (ASPE-LC-Q-TOF / MS) was established. Samples were extracted by HLB SPE and separated on Eclips Plus C18 reversed-phase column. The detection limit of zopiclone was 0.3μg / L and the concentration of zopiclone was 1 ~ 500μg / L with good linearity (R2 = 0.9993). The recovery of zopiclone in blood was over 70% Daytime RSD is not higher than 7.7%. The database of zopiclone was established by Agilent MassHunter PCDL Manager software, and the spiked samples were screened. The sample was added with zopiclone with a retention time deviation of 0.002 min, a mass deviation of 0.05 mDa, isotope peak shape matching score greater than 98, isotope Pitch score greater than 99, MS / MS map matching score greater than 94. Methods can be used for forensic and clinical analysis of poisons.