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作 者:张梦琪[1] 贾晶莹[1] 陆晓佩 陆川[1] 曹维锷[3] 李水军[1] 刘罡一[1] 余琛[1]
机构地区:[1]上海市徐汇区中心医院中心实验室,上海200031 [2]上海医药临床研究中心分析化学部,上海200233 [3]上海市徐汇区中心医院心内科,上海200031
出 处:《中国药学杂志》2011年第1期57-60,共4页Chinese Pharmaceutical Journal
基 金:上海市科委科研计划项目(08411966700)资助
摘 要:目的建立LC-MS/MS测定人血清中氯氮平、氟哌啶醇、洛沙平、利培酮、泰必利、西酞普兰、氟伏沙明、米安色林、米氮平、吗氯贝胺、帕罗西汀、瑞波西汀、曲唑酮、文拉法辛血药浓度的方法。方法血清经乙腈直接沉淀,采用伐地那非作为内标进行测定。色谱柱:XbridgeTM Phenyl(2.1mm×150 mm,5μm,Waters公司),流动相:0.02%甲酸水溶液-0.02%甲酸乙腈溶液(60∶40),等度洗脱;流速0.3mL·min-1;进样体积3μL;电喷雾离子化,正离子MRM扫描。结果氯氮平、西酞普兰、氟伏沙明、米安色林、米氮平、吗氯贝胺、瑞波西汀、曲唑酮、文拉法辛线性范围均为10~1000 ng·L-1(r>0.996),定量下限均为10ng·L-1;氟哌啶醇、利培酮、泰必利线性范围均为1~100ng·L-1(r>0.997),定量下限均为1ng·L-1;洛沙平、帕罗西汀线性范围均为5~500 ng·L-1(r>0.998),定量下限均为5ng·L-1;平均提取回收率均>87%,批内、批间精密度RSD均<15%。结论本方法灵敏度高、专一性好、操作简单,适用于5种抗精神类药物和9种抗抑郁药物的研究。OBJECTIVE To develop a LC-MS/MS method for the determination of clozapine,haloperidol,loxapine,risperidone,tiapride,citalopram,fluvoxamine,mianserin,mirtazapine,moclobemide,paroxetine,reboxetine,trazodone and venlafaxine in human serum.METHODS The serum samples were precipitated with acetonitrile.The internal standard was vardenafil.The analytical column was Xbridge^TM Phenyl(2.1 mm×150 mm,5 μm,Waters).The mobile phase consisted of 0.02% formic acid water-0.02% formic acid acetonitrile(60∶40),at the flow rate of 0.3 mL·min-1.The injection volume was 3 μL.The protonated ions of analytes were detected in positive ionization by multiple reactions monitoring(MRM) mode.RESULTS The linear ranges of clozapine,citalopram,fluvoxamine,mianserin,mirtazapine,moclobemide,reboxetine,trazodone and venlafaxine were validated from 10 to 1 000 ng· L^-1(r〉0.996)in plasma,and the low limits of quantitation was 10 ng· L^-1.The linear ranges of haloperidol,risperidone and tiapride were validated from 1 to 100 ng· L^-1(r〉0.997)in plasma,and the low limits of quantitation were 1 ng· L^-1.The linear ranges of loxapine and paroxetine were validated from 5 to 500 ng· L^-1(r〉0.998)in plasma and the low limits of quantitation were 5 ng·L^-1.The extraction recovery for all analytes was above 87%.The intra-and inter-batch precisions(RSD) were all less than 15%.CONCLUSION The established LC-MS/MS method is shown to be sensitive,accurate,simple and suitable for the research of five antipsychotics and nine antidepressants.
关 键 词:抗精神类药物 抗抑郁药物 液相色谱-串联质谱法 血清
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