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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 a Q-C18(2.1×50 mm,2.6μm),流动相为乙腈和0.5%甲酸水溶液,梯度洗脱,柱温30℃,进样量5μL,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 method for the determination of melatonin in peony by HPLC-MS / MS, and extract the melatonin from the peony samples with ultrasonic methanol. Chromatographic conditions: the column was Thermo a Q-C18 (2.1 × 50 mm, 2.6μm), the mobile phase was acetonitrile and 0.5% formic acid aqueous solution, gradient elution, column temperature 30 ℃, injection volume 5μL, flow rate 0.4 mL / min . Mass spectrometry conditions: electrospray positive ion mode (ESI +) ionization, multiple reaction monitoring mode (MRM) detection, the detected ion pairs m / z 233.2 → m / z 174.2,233.2 → m / z 159.2. Melatonin was well separated and detected within 25 min. The melatonin showed a good linear relationship in the range of 2 ~ 200 ng / mL. The RSDs of precision, repeatability and stability were all less than 10% Rates ranged from 64.87% to 74.59% with an average recovery of 70.06%. The method has high sensitivity, specificity and reliable and accurate results, and can provide an efficient and accurate detection method for the determination of melatonin in different tissues of Paeonia lactiflora.