高效液相色谱-电喷雾串联质谱法直接测定蜂蜜中脯氨酸  

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

作　　者：丁涛[1] 吕辰[2] 袁芳[1] 沈崇钰[1] 吴斌[1] 费晓庆[1] 陈国松[2] 张睿[1] 张晓燕[1] 陈磊[1] 袁娟[1] 庾金良[2] 李丽[3] 

机构地区：[1]江苏出入境检验检疫局食品实验室,南京210001 [2]南京工业大学理学院,南京211816 [3]桂林理工大学化学与生物工程学院,桂林541004

出　　处：《中国蜂业》2013年第11期41-43,48,共4页Apiculture of China

基　　金：质检总局项目2011IK218和2011IK209

摘　　要：建立了高效液相色谱-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-电喷雾串联质谱进行分析检测。以Phenomenex C18(100 mm×4.6mm×2.6μm)色谱柱为分析柱,乙腈和0.1%(v/v)甲酸-5 mmol/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25 mg/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100 mg/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。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.

关 键 词：脯氨酸 蜂蜜 高效液相色谱-电喷雾串联质谱 

分 类 号：S896.1[农业科学—特种经济动物饲养] O657.63[农业科学—畜牧兽医]