超高效液相色谱-高分辨质谱法测定蜂蜜中的苯甲酸、山梨酸、安赛蜜与糖精钠

Determination of Benzoic Acid,Sorbic Acid,Acesulfame-K and Saccharin Sodium in Honey by Ultra High Performance Liquid Chromatography-High Resolution Mass Spectrometry

建立了蜂蜜中苯甲酸、山梨酸、安赛蜜、糖精钠的超高效液相色谱-高分辨质谱分离测定方法。样品采用甲醇-水溶液（10∶90）提取，Diamonsil Plus C18色谱柱进行色谱分离，以0.5 mmol/L乙酸铵溶液和甲醇为流动相梯度洗脱，通过高分辨负离子扫描模式进行定性，外标法定量。结果表明，4种物质在0.02~2.0 mg/L范围内均具有良好的线性关系，相关系数为0.998 7~0.999 7。苯甲酸、山梨酸的方法定量下限为0.5 mg/kg，安赛蜜、糖精钠为0.3 mg/kg 。在低、中、高3个加标浓度下，方法的回收率为89.0%~104.0%，相对标准偏差（RSD）为2.0%~7.9%。该方法灵敏、简单、快速，定性准确可靠，适用于大批量蜂蜜中苯甲酸、山梨酸、安赛蜜、糖精钠的检测。

A method based on ultra high performance liquid chromatography-high resolution mass spectrometry was developed to separate benzoic acid，sorbic acid，acesulfame-K and saccharin sodium in honey.The targeted compounds in honey samples were extracted with methanol-water mixtures（10∶90）,and separated on a Diamonsil Plus C18 column with 0.5 mmol/L ammonium acetate-methanol as mobile phase by gradient elution.The qualitative and quantitative analyses were operated under t-MS2 by high resolution mass spectrometry with the external standard method.The results indicated that four analytes had good linearities in the concentration range of 0.02-2.0 mg/L with correlation coefficients of 0.998 7-0.999 7.The quantilition limits for benzoic acid，sorbic acid,acesulfame-K and saccharin sodium were 0.5，0.5，0.3,0.3 mg/kg，respectively.The recoveries of four compounds at three spiked levels were in the range of 89.0%-104.0%，with relative standard deviations（RSDs） of 2.0%-7.9%.The method was simple and rapid，and was suitable for the determination of benzoic acid，sorbic acid and acesulfame-K，saccharin sodium in honey.