摘要
建立了血液中抗抑郁类药物快速筛查的自动固相萃取-液相色谱-飞行时间质谱（ASPE-LC-Q-TOF/MS）方法。样品经HLB固相萃取柱提取后,采用LC-Q-TOF/MS进行测定,外标法定量。结果表明：目标物的线性范围为1-500μg/L,相关系数为0.997 6-0.999 7,检出限为0.01-0.5μg/L。在10、100和500μg/L3个添加水平的平均回收率为79.6%-96.4%,相对标准偏差为4.1%-6.4%。利用Agilent MassHunter PCDL Manager软件建立了抗抑郁类药物数据库,并应用于加标样品的筛查分析,本方法能够全部筛查出样品中添加的抗抑郁类药物,鉴定准确度达到100%,且保留时间偏差均小于0.1 min,质量偏差均小于1 mDa,同位素丰度匹配得分、同位素间距得分和MS匹配得分均大于95,MS/MS图谱匹配得分均大于70。利用本方法对实际案例进行筛查分析,检出阿米替林、卡马西平和多虑平,说明该方法可用于法庭与临床毒物分析。
A high-throughput method was developed for screening antidepressants in blood by automated solid phase extraction and liquid chromatography with high resolution quadrupole-time-offlight mass spectrometry（ASPE-LC-Q-TOF/MS）.The samples were cleaned up by an HLB solid phase extraction cartridge and analyzed by LC-Q-TOF/MS under electrospray ionization（ESI）mode with scanning range of m/z 50-1 000 Da.The chromatographic separation was performed on an Agilent Eclipse Plus C18column（50 mm×2.1 mm,1.8μm）with gradient elution using methanol and 5 mmol/L ammonium formate aqueous solution（containing 0.2% formic acid）as mobile phases.Rapid screening and confirmation can be achieved using MS matching scores,deviation of retention time,measured mass,isotopic abundance matching scores,isotope space matching scores and MS/MS matching scores.The quantitative analysis was carried out by correlating the extracting peak area with accurate mass.Good linearities were observed in the range of 1-500μg/L with the correlation coefficients from0.997 6 to 0.999 7.The limits of detection were 0.01-0.5μg/L.The spiked recoveries were 79.6%-96.4% with the relative standard deviations of 4.1%-6.4%.The result screening database was built using Agilent MassHunter PCDL Manager softwareand then used for the analysis of spiked samples.MS matching scores,isotopic abundance matching scores,isotope space matching scores（all95 points）and MS/MS matching scores（〉70 points）were applied to identify the analytes.The results showed that all the spiked antidepressants could be correctly identified with low deviation of retention time（〈0.1 min）and mass（〈1 mDa）.The developed method was further applied for the analysis of poisoning cases,and amitriptyline,carbamazepine,doxepin were detected.In brief,the method is rapid,sensitive,simple,reliable,and suitable for the screening and confirmation of antidepressants in forensic and clinical analytical toxicology.
出处
《色谱》
CAS
CSCD
北大核心
2014年第7期687-692,共6页
Chinese Journal of Chromatography
基金
重庆市公安局科技攻关计划项目(G2013-04)
关键词
自动固相萃取
液相色谱
飞行时间质谱
抗抑郁类药物
血液
筛查
确证
automated solid phase extraction（ASPE）
liquid chromatography（LC）
time-of-flight mass spectrometry（TOF/MS）
antidepressants
blood
screening
confirmation
