蜂胶中咖啡酸苯乙酯的测定.docVIP

液相色谱-串联质谱法测定蜂胶中的咖啡酸苯乙酯 李丽1,2，吴俐勤2，章虎2，莫卫民1，王方莉1,2，陈志民2，钱鸣蓉2* （1.浙江工业大学化学工程与材料学院， 杭州310014；2.浙江省农业科学院农产品质量标准研究所杭州310021=（80:20，V/V离子对m/z 238/135.0和238/179.0用于定性，m/z 238/135.0用于定量~500.0 μg·L-1范围内呈线性关系良好，相关系数为0.9948。在0.01、0.1、1.0 g·kg-1加标水平下方法的回收率为94.0%~98.6%，相对标准偏差（RSD）在2.5%~3.5%之间，方法的检出限为0.003 g·kg-1，则定量限为0.01 g·kg-1。采用该方法检测24个蜂胶样品，咖啡酸苯乙酯的平均含量在0.0394~15.8g·kg-1范围内，相对标准偏差为1.5%~7.4%。该方法快速、准确、灵敏，可有效用于蜂胶中咖啡酸苯乙酯的质量控制。 关键词：蜂胶；咖啡酸苯乙酯；高效液相色谱-串联质谱法 中图分类号：0657.63 文献标志码：A Determination of phenethyl caffeate in propolis by High Performance Liquid Chromatography-Tandem Mass Spectrometry LI li1,2，WU Li-qin2，ZHANG Hu2，MO Wei-min1，WANG Fang-li1,2，CHEN Zhi-min2，QIAN Ming-rong2* (1.Zhejiang university of technology, Hangzhou 310014；2.Institute of Quality and Standard on Agricultural Products, Zhejiang Academy of Agricultural Sciences, Hangzhou 310021；) Abstract：A high performance liquid chromatography-tandem mass spectrometric(HPLC-MS/MS) method was developed for the determination of phenethyl caffeate in propolis. After the sample was extracted with methanol, the supernatant fluid was transferred and diluted. The separation of analysis was made on a C18 chromatographic column using acidulated methanol-ammonium acetate solution (80: 20,V：V) as mobile phase. The sample was determined by tandem mass spectrometry under the multiple reaction monitoring in negative anion and quantified by external standard calibration. Ion of m/z 238.1/135.0 and 238.1/135.0 for qualitative, 238.1/135.0 m/z was used to quantitatively.Result showed that the calibration curve of phenethyl caffeate was linear in the range of 0.2~500.0 μg·L-1 with a correlation coefficient of 0.9948. The recoveries for phenethyl caffeate at three spiked levels (0.01,0.1,1.0g·kg-1) were in the range of 94.0%-98.6% with relative standard deviations (RSDs, n=5) of 2.5%~3.5%, the limits of detection and limits of quantitation were 0.003 g·kg-1 and 0.01 g·kg-1, respectively. The method was applied in the detection of phen