UPLC-MS/MS测定安神类中成药和保健食品中8种非法添加抗抑郁类化学成分
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摘要
目的建立了安神类中成药和保健食品中的8种非法添加抗抑郁类化学成分的超高效液相色谱-三重四级杆串联质谱(UPLC-MS/MS)检测方法。方法以甲醇为提取溶剂,Waters ACQUITY UPLC BEH C_(18)(2.1 mm×100 mm,1.7μm)色谱柱分离,三重四级杆质谱仪检测,MRM模式定性、定量检测安神类中成药和保健食品中的8种抗抑郁类化学成分(文拉法辛、西酞普兰、帕罗西汀、阿米替林、氟西汀、三甲丙咪嗪、舍曲林和氯丙咪嗪)。结果 8种抗抑郁类化学成分质谱检测的线性范围宽,相关性好,r≥0.9955;方法精密度RSD为1.5%～4.6%;方法回收率为88.2%～103.2%;定量限为0.02～0.03μg·L~(-1);日内精密度的RSD(n=5)为1.1%～3.8%,日间精密度的RSD(n=9)为1.4%～3.7%。结论本方法专属性强,操作简单,快捷,可作为安神类中成药和保健食品中8种抗抑郁类化学成分定量、定性的有效检测方法。
OBJECTIVE To develop a ultra performance liquid chromatography coupled with triple quadrupole mass spectrometry(UPLC-MS/MS) method to determine 8 antidepressants in tranquilizing traditional Chinese medicine and health food. METHODS The analysis was performed by a UPLC-MS/MS system with Waters ACQUITY UPLC BEH C_(18)(2.1 mm×100 mm, 1.7 μm) column. Multiple-reaction monitoring(MRM) was performed to identify and quantify 8 antidepressants(venlafaxine, citalopram, paroxetine, amitriptyline, trimepramine, fluoxetine, sertraline and clomipramine), which were extracted from samples with methanol. RESULTS Linear calibration curves were obtained with r≥0.995 5. The precision of the method was showed by RSDs(n=6) ranging from 1.5% to 4.6%. The recoveries were determined at three concentration levels and ranged from 88.2% to 103.2%. The ranges of LOQs were from 0.02 to 0.03 μg·L~(-1) and the RSDs(n=9)of intra-day precision and inter-day precision were from 1.1% to 3.8% and from 1.4% to 3.7%, respectively. CONCLUSION The method is specific, simple and rapid to detect 8 antidepressants in tranquilizing traditional Chinese medicine and health food.
OBJECTIVE To develop a ultra performance liquid chromatography coupled with triple quadrupole mass spectrometry(UPLC-MS/MS) method to determine 8 antidepressants in tranquilizing traditional Chinese medicine and health food. METHODS The analysis was performed by a UPLC-MS/MS system with Waters ACQUITY UPLC BEH C_(18)(2.1 mm×100 mm, 1.7 μm) column. Multiple-reaction monitoring(MRM) was performed to identify and quantify 8 antidepressants(venlafaxine, citalopram, paroxetine, amitriptyline, trimepramine, fluoxetine, sertraline and clomipramine), which were extracted from samples with methanol. RESULTS Linear calibration curves were obtained with r≥0.995 5. The precision of the method was showed by RSDs(n=6) ranging from 1.5% to 4.6%. The recoveries were determined at three concentration levels and ranged from 88.2% to 103.2%. The ranges of LOQs were from 0.02 to 0.03 μg·L~(-1) and the RSDs(n=9)of intra-day precision and inter-day precision were from 1.1% to 3.8% and from 1.4% to 3.7%, respectively. CONCLUSION The method is specific, simple and rapid to detect 8 antidepressants in tranquilizing traditional Chinese medicine and health food.
引文
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[14]GOU X L,GAO X,HU G H,et al.Simultaneous determination of nine antidepressants in traditional Chinese medicines and health food by ultra performance liquid chromatography with tandem mass spectrometry[J].Chin JChromatogr(色谱),2014,32(8):822-826.
[15]MING D S,HEATHCOTEA J.A rapid and accurate UPLC/MS/MS method for the determination of benzodiazepines in human urine[J].J Chromatogr B,2011,879(5/6):421-428.
[16]CHAMBERS E E,WOODCOCK M J,WHEATON J P,et al.Systematic development of an UPLC-MS/MS method for the determination of tricyclic antidepressants in human urine[J].JPharm Biomed,2014(88):660-665.
[2]GAO J B,LI Y D,YANG S Z,et al.Impact of Yixinshu capsules on quality of life,anxiety and depression of coronary heart disease patients after PCI[J].Chin J New Drugs(中国新药杂志),2017,26(10):56-59.
[3]ZHOU X L,LIN Y,ZHENG G Q.Therapeutic progress of mental diseases(second):depression[J].Her Med(医药导报),2017,36(10):1137-1142.
[4]HUANG X W,HUANG Q T,PAN J Y.Clinical application of antidepressants in the treatment of insomnia symptoms[J].Chin J Contemp Neurol Neurosurg(中国现代神经疾病杂志),2013,13(11):971-975.
[5]HOLDEN C.Global survey examines impact of depression[J].Science,2000,288(5463):39-40.
[6]LI Y X,WANG H H.Efficacy of antidepressants in the treatment of patients with functional dyspepsia:a meta-analysis[J].Chin J Drug Eval(中国药物研究),2012,29(1):35-40.
[7]GAO L W,MA X T,YU L X,et al.Determination of amitriptyline in rat blood and urine by gas chromatography[J].Chin J Forensic Med(中国法医学杂志),2011,26(2):127-129.
[8]FERNáNDEZ P,GONZáLEZ C,PENA M T,et al.A rapid ultrasound-assisted dispersive liquid-liquid microextraction followed by ultra-performance liquid chromatography for the simultaneous determination of seven benzodiazepines in human plasma samples[J].Anal Chim Acta,2013(767):88-96.
[9]CARTISER N,BéVALOT F,LE MEUR C,et al.Gas chromatography-tandem mass spectrometry assay for the quantification of four benzodiazepines and citalopram in eleven postmortem rabbit fluids and tissues,with application to animal and human samples[J].J Chromatogr B,2011,879(27):2909-2918.
[10]VARDAKOU I,DONA A,PISTOS C,et al.Validated GC/MS method for the simultaneous determination of clozapine and norclozapine in human plasma.Application in psychiatric patients under clozapine treatment[J].JChromatogr B,2010,878(25):2327-2332.
[11]WU H Q,JIN Y C,CAI M Z,et al.Smiultaneous determination of 10 mental drugs by gas chromatography-mass spectrometry[J].Chin J Anal Chem(分析化学),2007,35(4):500-504.
[12]GUO J Q,SHI Y T,WANG H J,et al.Simultaneous determination of 5 antidepressants in blood by automated solid phase extraction and liquid chrommatography-tandem mass spectrometry[J].Chin J Anal Chem(分析化学),2014,42(5):701-705.
[13]LIU G R,QIAO S,YU YH Y,et al.Simultaneous determination of nine antidepressants in human plasma by UPLC-MS/MS[J].Chin J Clin Pharmacol(中国临床药理学杂志),2016,32(23):2191-2194.
[14]GOU X L,GAO X,HU G H,et al.Simultaneous determination of nine antidepressants in traditional Chinese medicines and health food by ultra performance liquid chromatography with tandem mass spectrometry[J].Chin JChromatogr(色谱),2014,32(8):822-826.
[15]MING D S,HEATHCOTEA J.A rapid and accurate UPLC/MS/MS method for the determination of benzodiazepines in human urine[J].J Chromatogr B,2011,879(5/6):421-428.
[16]CHAMBERS E E,WOODCOCK M J,WHEATON J P,et al.Systematic development of an UPLC-MS/MS method for the determination of tricyclic antidepressants in human urine[J].JPharm Biomed,2014(88):660-665.