高效液相色谱-三重四级杆/复合线性离子阱质谱测定鼠脑组织中神经甾体类化合物
建立了高效液相色谱-串联质谱法(HPLC-MS/MS)测定鼠脑组织中6种神经甾体类激素(别孕烯醇酮、孕烯醇酮、孕酮、脱氧皮质酮、四氢脱氧皮质酮、去氢表雄酮)的方法。采用Agilent XDB-C18色谱柱,以5 mmol/L乙酸铵-甲醇为流动相,梯度洗脱分离,在电喷雾正离子模式下,以多反应监测(MRM)扫描模式采集数据,基质匹配内标法定量。孕酮和脱氧皮质酮在0.10~10 ng/m L范围内呈良好的线性关系,别孕烯醇酮、孕烯醇酮、四氢脱氧皮质酮、去氢表雄酮在0.50~10 ng/m L范围内呈良好的线性关系,相关系数均大于0.99;在0.4,4.0和8.0 ng/m L加标水平下的平均回收率为...
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Published in | 分析化学 Vol. 43; no. 8; pp. 1118 - 1124 |
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Main Author | |
Format | Journal Article |
Language | Chinese |
Published |
北京大学系统生物医学研究所,北京,100191%北京大学神经科学研究所,北京,100191%中国人民解放军白求恩国际和平医院药学部,石家庄,050082
2015
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Subjects | |
Online Access | Get full text |
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Summary: | 建立了高效液相色谱-串联质谱法(HPLC-MS/MS)测定鼠脑组织中6种神经甾体类激素(别孕烯醇酮、孕烯醇酮、孕酮、脱氧皮质酮、四氢脱氧皮质酮、去氢表雄酮)的方法。采用Agilent XDB-C18色谱柱,以5 mmol/L乙酸铵-甲醇为流动相,梯度洗脱分离,在电喷雾正离子模式下,以多反应监测(MRM)扫描模式采集数据,基质匹配内标法定量。孕酮和脱氧皮质酮在0.10~10 ng/m L范围内呈良好的线性关系,别孕烯醇酮、孕烯醇酮、四氢脱氧皮质酮、去氢表雄酮在0.50~10 ng/m L范围内呈良好的线性关系,相关系数均大于0.99;在0.4,4.0和8.0 ng/m L加标水平下的平均回收率为91.2%~115.5%;相对标准偏差(RSD,n=6)为0.87%~8.8%;检出限为0.04~0.20 ng/m L,定量限为0.10~0.50 ng/m L。 |
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Bibliography: | LIU Jia, ZHANG Meng, WAN You, WU Hong-Hai, HOU Yan-Ning, ZHENG Le-Min, YIN Yu-Xin 1( Institute of Systems Biomedicine, Peking University Health Science Center, Beijing 100191, China) 2 ( Neurosctence Research Institute, Peking University, Beijing 100191, China) 3 ( Bethune International Peace Hospital, Shijiazhuang 050082, China) 22-1125/O6 Neurosteroids; Liquid chromatography-tandem mass spectrometry; Multiple reaction monitoring; Rat brain An analytical method based on high performance liquid chromatography tandem mass spectrometry was developed for the simultaneous determination of 6 neurosteroids in rat brain tissues. The neurosteroids were separated on an Agilent XDB-Cls column (50 mm×4.6 mm, 1.8 μm), using methanol-5 mmol/L ammonium acetate as the mobile phase. A gradient elution program with a cycle time of 10 min was used. The neurosteroids were detected by electrospray ionization mass spectrometry in positive mode with multiple reaction monitoring (MRM) scan mode. For ll-deoxycorticosterone (DOC) and pr |
ISSN: | 0253-3820 |
DOI: | 10.11895/j.issn.0253-3820.150149 |