分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2014年
5期
701-705
,共5页
郭璟琦%石银涛%王绘军%张盼%郑经%王俊伟
郭璟琦%石銀濤%王繪軍%張盼%鄭經%王俊偉
곽경기%석은도%왕회군%장반%정경%왕준위
抗抑郁药%液相色谱-串联质谱%自动固相萃取%血液
抗抑鬱藥%液相色譜-串聯質譜%自動固相萃取%血液
항억욱약%액상색보-천련질보%자동고상췌취%혈액
Antidepressants%Liquid chromatography-tandem mass spectrometry%Automated solid phase extraction%Blood
建立了血液中5种抗抑郁类药物的自动固相萃取-液相色谱-串联质谱( ASPE-LC-MS/MS)分析方法。样品经HLB固相萃取柱提取后,采用LC-MS/MS进行测定,外标法定量。在Waters AtlantisTM dC18反相柱上分离,梯度洗脱,流动相为甲醇-0.1%甲酸(1:4, V/V)溶液,质谱采集为电喷雾正离子多反应监测模式。采用基质匹配标准溶液校正,5种目标物在1~500μg/L范围内具有良好的线性关系,相关系数( R)大于0.9975,检出限在0.1~0.6μg/L之间;添加浓度水平为10,100和500μg/L时,方法回收率为70.6%~93.8%,相对标准偏差在3.9%~9.2%之间。本方法可用于血液中5种抗抑郁类药物的法庭与临床毒物分析。
建立瞭血液中5種抗抑鬱類藥物的自動固相萃取-液相色譜-串聯質譜( ASPE-LC-MS/MS)分析方法。樣品經HLB固相萃取柱提取後,採用LC-MS/MS進行測定,外標法定量。在Waters AtlantisTM dC18反相柱上分離,梯度洗脫,流動相為甲醇-0.1%甲痠(1:4, V/V)溶液,質譜採集為電噴霧正離子多反應鑑測模式。採用基質匹配標準溶液校正,5種目標物在1~500μg/L範圍內具有良好的線性關繫,相關繫數( R)大于0.9975,檢齣限在0.1~0.6μg/L之間;添加濃度水平為10,100和500μg/L時,方法迴收率為70.6%~93.8%,相對標準偏差在3.9%~9.2%之間。本方法可用于血液中5種抗抑鬱類藥物的法庭與臨床毒物分析。
건립료혈액중5충항억욱류약물적자동고상췌취-액상색보-천련질보( ASPE-LC-MS/MS)분석방법。양품경HLB고상췌취주제취후,채용LC-MS/MS진행측정,외표법정량。재Waters AtlantisTM dC18반상주상분리,제도세탈,류동상위갑순-0.1%갑산(1:4, V/V)용액,질보채집위전분무정리자다반응감측모식。채용기질필배표준용액교정,5충목표물재1~500μg/L범위내구유량호적선성관계,상관계수( R)대우0.9975,검출한재0.1~0.6μg/L지간;첨가농도수평위10,100화500μg/L시,방법회수솔위70.6%~93.8%,상대표준편차재3.9%~9.2%지간。본방법가용우혈액중5충항억욱류약물적법정여림상독물분석。
An efficient and accurate analytical method was developed for the simultaneous determination of 5 antidepressants in blood, by automated solid phase extraction-liquid chromatography tandem mass spectrometry ( ASPE-LC-MS/MS) . The samples were cleaned up by HLB solid phase extraction cartridge, and the analyses were carried out on LC-MS/MS. The chromatographic separation was performed on a Waters AtlantisTM dC18 column with gradient elution by using methanol and formic acid in water as mobile phases. Detection was carried out under the multiple reaction monitoring ( MRM) in positive ionization mode. Matrix-matched calibration curves with good correlation coefficients ( R>0 . 9975 ) were obtained in the concentration range of 1-500 μg/L. The detection limits of the method were 0. 1-0. 6 μg/L. The mean recoveries at the three spiked levels of 10-500 μg/L were 70 . 6%-93 . 8%, and the relative standard deviations were 3 . 9%-9. 2%. The method is applicable to analyze antidepressants in forensic and clinical toxicology.