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建立高效液相色谱-串联质谱(HPLC-MS/MS)专一性测定芍药褪黑素含量的检测方法,采用超声波甲醇提取芍药样品中的褪黑素.色谱条件:色谱柱为Thermo aQ-C18 (2.1×50 mm,2.6 μm),流动相为乙腈和0.5%甲酸水溶液,梯度洗脱,柱温30℃,进样量5 μL,流速0.4 mL/min.质谱条件:电喷雾正离子模式(ESI+)电离,多反应监测模式(MRM)检测,检测离子对为m/z 233.2--→m/z 174.2、233.2→m/Z 159.2.在25 min内褪黑素得到很好的分离并被检测,褪黑素在2~200 ng/mL范围内呈良好的线性关系、精密度、重复性和稳定性的RSD均小于10%,回收率在64.87%~74.59%之间,平均回收率70.06%.本方法灵敏度高、专一性强、结果可靠准确,可为测定芍药不同组织中褪黑素含量提供一种高效精准的检测方法.“,”To establish a HPLC-MS/MS method to determine the contents of melatonin with multi-reactions monitoring (MRM) technology in different organs of Paeonia laetiflora Pall.and melatonin was extracted from samples with methanol under the assistance of ultrasonic.The HPLC condition was as follows:separation column:Thermo aQ-C18 column (2.1×50 ram,2.6 μm);mobile phase,acetonitrile-0.5% methanoic acid solution with gradient elution;injection volume:5 μL;flow rate:0.4 mL/min;column temperature:30℃C.Mass spectrometric conditions:the electrospray was operated under the positive ionization mode and the drug was identified by multiple reaction monitoring (MRM) mode.The ion of monitor was at m/z 233.2→rn/z 174.2 and m/z 233.2→m/z 159.2.Melatonin was well separated and detected in 25 minutes and the melatonin standards represented a good linear relationship with the range of 2~200 ng/mL.The recovery varied from 64.87% to 74.59% and the average recovery was 70.06%.The relative standard deviration was lower than 10%.Conclusion:The method has high sensitivity,better specificity and accurate results which can be a high-efficiency and accurate method for the determination of melatonin in Paeonia lactiflora Pall..