Quantitative determination of forty-eight antidepressants and antipsychotics in human serum by HPLC tandem mass spectrometry:: A multi-level, single-sample approach
Quantitative determination of forty-eight antidepressants and antipsychotics in human serum by HPLC tandem mass spectrometry:: A multi-level, single-sample approach
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DOI：
10.1016/j.jchromb.2006.05.031
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发表时间：
2006-10-20
影响因子：
3
通讯作者：
Kuehn-Velten, W. N.
中科院分区：
文献类型：
--
作者：
Kirchherr, H.;Kuehn-Velten, W. N.
建立了同时测定阿米舒利、阿米替林、阿立哌唑、苯哌利多、氯丙氨嗪、氯丙咪嗪、氯丙咪嗪、氯氮平、地昔帕明、多塞平、氟西汀、氟哌啶、氟哌嗪、氟伏沙明、氟哌啶醇、羟利培酮、丙咪嗪、左美沙星、马普替林、米安色林、米氮平、吗氯贝胺、去甲氯普胺、去甲氧西平、去甲氧西平、去甲氧西林、去甲万乃馨、去甲万乃静、氟西汀、氟西汀、帕罗西汀、安定、奋乃静、吡哌酮、安培酮、奎尼替林、瑞博西汀、马普替林、米安色林、米氮平、吗氯贝胺、去甲氯普胺、去甲氧西汀、去甲氧西汀、去甲万拉平、哌嗪、哌嗪、安培酮、奎硫平、瑞波西汀、舒马西林、舒拉西林、曲拉维酮、甲硝唑通过进一步稀释第一次蛋白质沉淀后获得的上清液，将药物分成低、中、高三个亚组(考虑的总治疗水平范围：0.5-2000 ng/mL)。色谱柱为C18色谱柱(50 nm×4.6 mm)，甲醇梯度洗脱，5 MM醋酸盐缓冲液，pH 3.9。注射间隔时间为8min。一套由三个内部标准组成的标准用于对疏水性差异很大的药物进行定量。电喷雾电离后，用API4000串联质谱仪在多反应监测(MRM)模式下检测正离子碎片。回归参数的校正曲线和定量限显示良好的覆盖治疗和亚治疗范围，平均相关系数为0.9988。在所有亚组的三个浓度范围内，都准备了不精密度和不精确度测量用于试剂盒内和试剂间的比较。批内和批间比较的平均变异系数分别为6.1%和7.4%，而与添加浓度的平均偏差分别为4.8%和4.2%。回收率，用添加的血清样本相对于不含血清基质的标准溶液的百分比回收率来衡量，在92%到111%之间变化，平均为101%。作为唯一例外，奥氮平在血清基质中的有效率(185%)远远高于无基质对照组。(C)2006爱思唯尔B.V.保留所有权利。
This method describes the simultaneous determination of amisulpride, amitriptyline, aripiprazole, benperidol, chlorpromazine, chlorprothixene, citalopram, clomipramine, clozapine, desipramine, doxepin, fluoxetine, flupentixol, fluphenazine, fluvoxamine, haloperidol, hydroxyrisperidone, imipramine, levomepromazine, maprotiline, mianserine, mirtazapine, moclobemide, norclomipramine, nordoxepin, norfluoxetine, nortriptyline, O-desmethylvenlafaxine, olanzapine, opipramol, paroxetine, perazine, perphenazine, pimozide, pipamperone, quetiapine, reboxetine, risperidone, sertraline, sulpiride, thioridazine, trazodone, trimipramine, venlafaxine, viloxazine, ziprasidone, zotepine and zuclopenthixol with a single sample/triple injection approach. Drugs were assigned to subgroups covering low, medium and high concentrations (overall range of therapeutic levels to be considered: 0.5-2000 ng/mL) by further dilution of the supernatant obtained after the first protein precipitation. Chromatographic separation was necessary for isobaric mass fragments and performed on a monolithic C 18 column (50 nun x 4.6 mm) with methanol gradient and 5 MM acetate buffer at pH 3.9. The injection interval was 8 min. A set of three internal standards was used for quantification of drugs with widely varying hydrophobicity. After electrospray ionization positive ion fragments were detected in the multiple reaction monitoring (MRM) mode with an API 4000 tandem mass spectrometer. Regression parameters of calibration curves and limits of quantification showed good covering of therapeutic and subtherapeutic ranges with an average correlation coefficient of 0.9988. Imprecision and inaccuracy measures were prepared for intra- and inter-assay comparisons at three concentration ranges in all subgroups. Average coefficients of variation were 6.1% for intra-assay and 7.4% for inter-assay comparisons, while average deviations from spiked concentrations were 4.8% for intra-assay and 4.2% for inter-assay comparisons, respectively. Recovery rates, measured as the percent recoveries of spiked serum samples against standard solutions without serum matrix, varied between 92 and 111%, with an average of 101%. As the only exception, the olanzapine response was much higher (185%) in serum matrix than in matrix-free controls. (c) 2006 Elsevier B.V. All rights reserved.