摘要
目的建立测定蝙蝠蛾被毛孢菌丝体中褪黑素含量的高效液相色谱-串联质谱方法。方法样品中褪黑素以甲醇为提取溶剂,以超声波为提取方式进行提取。采用色谱柱Thermo Beta Basic-18(150 mm×4.6 mm,5μm),流动相为甲醇-0.1%甲酸水(60∶40),流速0.6 ml/min,柱温40℃。用串联离子阱质谱在电喷雾电离正离子(ESI+)-二级质谱(MS/MS)模式进行质谱测定。结果方法的线性范围为10～200μg/kg,基质加标工作曲线线性方程为y=10204.8x-8575.85,相关系数r=0.999 2。方法的检出限为0.5μg/kg,定量限为2.0μg/kg,平均回收率为81.92%,相对标准偏差<10%。结论本方法选择性高、快速,可以应用于蝙蝠蛾被毛孢菌丝体粉末中褪黑素检测,也可为其他复杂体系中褪黑素的测定提供依据。
Objective To establish a method of determining melatonin in Cordyceps sinensis mycelium by high performance liquid chromatograhy eleetrospray inonization tendem mass spectrometry （HPLC-MS/MS）. Methods Melatonin in the sample was extracted utrasonically with methanol. The content was then seperated on Thermo Beta Basic- 18 column （ 150 mm×4. 6 mm, 5μm） with methanol/0. 1% formic acid solution （60： 40） as mobile phase. The flow rate was 0.6 ml/min, and column temperature was set to 40 ℃. Detection was performed under positive ion eleetrospray ionization tandem ion trap mass spectrometry （ESI ＋ ） -tandem mass spectrometry （MS/MS） mode. Results There was a good linearity of melatonin in the range of 10 - 200 μg/kg with correlation coefficient of O. 999 2. The detection limit of the method was 0. 5μg/kg, and the limit of the quantification was 2. 0 μg/kg. The averange recovery was 81.92%. The relative standard deviration was lower than 10%. Conelusion This method is selective and fast. It can be applied to detect the melatonin in Cordyceps sinensis mycelium powder, and it may also provide basis for the determination in other complex systems.
出处
《中国食品卫生杂志》
北大核心
2013年第2期162-165,共4页
Chinese Journal of Food Hygiene
