高效液相色谱-质谱法同时测定食品中5种单、双糖的含量

Simultaneous Determination of Monosaccharide and Disaccharide Contents in Foods by High Performance Liquid Chromatography-Mass Spectrometry

建立同时定性和定量分析食品中果糖、葡萄糖、蔗糖、麦芽糖、乳糖的检测方法——高效液相色谱-质谱法。样品经纯水旋转涡流提取,加入100mL乙腈去蛋白,过滤定容。采用ACQUITY BEH Amide色谱柱,以乙腈-水溶液(各含体积分数0.1%氨水)为流动相,在雾化气压力为0.69MPa、干燥气温度200℃、干燥气流速8mL/min条件下,应用电喷雾离子化四极杆串联质谱,选择负离子采集模式以反应离子监测(SIM)方式进行测定分析。结果表明,5种糖的检出限依次为果糖32μg/kg、葡萄糖32μg/kg、蔗糖9μg/kg、麦芽糖21μg/kg、乳糖20μg/kg。在添加水平为2～10g/kg范围内,回收率为98.5%～102.2%、相对标准偏差为0.2%～1.4%。该方法操作简单、灵敏度高、重现性好、结果准确可靠,可用于低糖或无糖食品中单、双糖含量的快速检测。

A high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） method was developed for the simultaneous determination of five saccharides such as fructose,glucose,sucrose,maltose and lactose in foods.Samples were extracted with water under rotating vortex field,and protein was removed by using 100 mL of acetonitrile.The extract was separated on an ACQUITY BEH Amide HPLC column using acetonitrile-water（both containing 0.1% ammonia） as mobile phase.The electrospray ionization tandem quadrupole mass spectrometric analysis was carried out in the negative ion mode using selective reaction-monitoring（SIM） under the conditions： 10 MPa nebulizer pressure,200 ℃ drying gas temperature,and 8 mL/min flow rate.The limits of detection were 32μg/kg for fructose,32μg/kg for glucose,9μg/kg for sucrose,21μg/kg for maltose and 20μg/kg for lactose.The average recovery rates were 98.5%-102.2% at 10 g/kg and 2 g/kg spike levels with a relative standard deviation of 0.2%-1.4%.This developed method is characteristics of rapidity,high sensitivity,precision and convenient operation,thereby providing a promising approach for simultaneous determination of trace sugars in foods.