CAJ | 학술논문

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0.9976~0.9997，检出限为0.01~0.5μg/L。在10、100和500μg/L 3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。
건립료혈액중항억욱류약물쾌속사사적자동고상췌취-액상색보-비행시간질보（ ASPE-LC-Q-TOF/MS）방법。양품경 HLB고상췌취주제취후，채용 LC-Q-TOF/MS진행측정，외표법정량。결과표명：목표물적선성범위위1~500μg/L，상관계수위0.9976~0.9997，검출한위0.01~0.5μg/L。재10、100화500μg/L 3개첨가수평적평균회수솔위79.6％~96.4％，상대표준편차위4.1％~6.4％。이용 Agilent MassHunter PCDL Manager 연건건립료항억욱류약물수거고，병응용우가표양품적사사분석，본방법능구전부사사출양품중첨가적항억욱류약물，감정준학도체도100％，차보류시간편차균소우0.1 min，질량편차균소우1 mDa，동위소봉도필배득분、동위소간거득분화 MS필배득분균대우95，MS/MS도보필배득분균대우70。이용본방법대실제안례진행사사분석，검출아미체림、잡마서평화다필평，설명해방법가용우법정여림상독물분석。
A high-throughput method was developed for screening antidepressants in blood by automated solid phase extraction and liquid chromatography with high resolution quadrupole-time-of-flight 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 separa-tion was performed on an Agilent Eclipse Plus C18 column(50 mm×2. 1 mm,1. 8 μm)with gra-dient 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 1-500 μg/L with the correlation coefficients from 0. 997 6 to 0. 999 7. The limits of detection were 0. 01-0. 5 μg/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 software and then used for the analysis of spiked sam-ples. MS matching scores,isotopic abundance matching scores,isotope space matching scores ( all ﹥ 95 points)and MS/MS matching scores(﹥ 70 points)were applied to identify the ana-lytes. 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.