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    快速溶剂萃取-气相色谱-串联质谱法测定血中12种催眠类药物

    Determination of 12 Hypnotics in Blood by GC-MS/MS with Accelerated Solvent Extraction

    • 摘要: 提出了气相色谱-串联质谱法测定血液中12种催眠类药物含量的方法.样品以乙酸乙酯-环己烷-丙酮(2+2+1)混合液为萃取剂,使用氧化铝吸附剂达到在线净化的效果,经快速溶剂萃取仪提取后,提取液用氮气吹干,用甲醇0.5 mL溶解,通过VF-5MS色谱柱分离,采用电子轰击离子源多反应监测模式进行测定.12种催眠类药物的质量浓度与其峰面积均在50.0~1 000 μg·L-1之间呈线性关系,测定下限(10S/N)在0.02~4.7 μg·L-1之间.加标回收率在65.4%~98.2%之间,测定值的相对标准偏差在0.9%~14.8%之间.

       

      Abstract: GC-MS/MS was applied to the determination of 12 hypnoticsin in blood. The sample was extracted with a mixture of ethyl acetate,cyclohexane and acetone (2+2+1) by accelerated solvent extraction,and purified using alumina powder online. The extract was then evaporated to dryness by N2-blowing and dissolved in 0.5 mL of methanol. A VF-5MS chromatographic column was used for separation. Electron impact was used for ionization source. MRM was adopted in MS. The linear relationships between the peak area and the mass concentration of 12 hypnotics was kept in the same range of 50.0-1 000 μg·L-1,with the lower limits of determination (10S/N) in the range of 0.02-4.7 μg·L-1. Recovery rates measured by standard addition were in the range of 65.4%-98.2%,with RSD in the range of 0.9%-14.8%.

       

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