高效液相色谱-电喷雾串联质谱法直接测定蜂蜜中脯氨酸

建立了高效液相色谱一电喷雾串联质谱法直接测定蜂蜜中脯氨酸的方法。蜂蜜样品用去离子水溶解后，过0．45μm水相微孔滤膜，高效液相色谱一电喷雾串联质谱进行分析检测。以Phenomenex C18（100mmx4．6mmx2．6μm）色谱柱为分析柱，乙腈和0．1％（v／v）甲酸-5mmol／L乙酸铵水溶液为流动相进行梯度洗脱，在电喷雾正离子多反应监测模式下进行检测，外标法定量。通过加标验证，该方法检测低限可达25mg／kg，脯氨酸在0．5～10．0μg／mL浓度范围内线性关系良好，相关系数大于0．99。在25、50和100mg/kg三个加标水平下，蜂蜜中脯氨酸平均回收率为83．7～109．6％，相对标准偏差（RSD）为2．4～10．9％。该方法样品处理简单、快速，结果准确，灵敏度高，可以作为日常蜂蜜中脯氨酸的检测方法。

Direct determination of proline in honey by liquid chromatography-electrospray ionization tandem mass spectrometry

A liquid chromatography-electrospray ionization tandem mass spectrometry （LC-MS/MS）method was developed for the determination of proline in honey. The honey samples were diluted with deionized water. The separation of analyte was carried out on a Phenomenex Cls column （100mm×4.6mm,2.61μm）using mobile phases of acetonitrile-5mmol/1 ammonium acetate- 0.1% （v/v）formic acid solution with gradient elution. The analysis was carried out by multi-reaction monitoring（MRM）mode with electrospray ionization interface（ESI）in positive mode. The calibration curve was good in the range of 0.5-10 μg/ml recoveries were between 83.7% to 109.6% at （r〉0.99）. The detection limit of the method was 25 mg/kg. The average three spiked levels （25 , 50 and 100 mg/kg） with the relative standard deviations （RSDs）no more than 10.9 % .The method is simple, rapid, and suitable to detect the proline in honey with high throughput.