高效液相色谱法测定食品中苯甲酸、山梨酸和糖精钠  

Determination of Benzoic Acid,Sorbic Acid and Sodium Saccharin in Food by High Performance Liquid Chromatography

作　　者：李鸿展 Li Hongzhan(Sichuan Environmental Protection Engineering Co.,Ltd.,CNNC,Guangyuan 628000,China)

机构地区：[1]中核四川环保工程有限责任公司,四川广元628000

出　　处：《广东化工》2023年第14期172-176,共5页Guangdong Chemical Industry

摘　　要：建立了同时测定苯甲酸、山梨酸和糖精钠3种食品添加剂的高效液相色谱法。在流动相为甲醇+0.02 mol/L乙酸铵溶液流动相体系中,通过引入冰醋酸来改变缓冲溶液的酸碱度、改变梯度洗脱比例,进而改善色谱峰分离的选择性。以ANPU-WP C18(250×4.6 mm,5μm)为分离柱,在230 nm测定波长下进行检测,设置流速1.0 m L/min,进样量20μL,甲醇:0.02 mmol/L乙酸铵溶液(pH=6.5)(10∶90,v∶v)为流动相,同时对缓冲溶液的pH以及流动相梯度洗脱程序进行优化。在优化后的最佳色谱条件下,苯甲酸、山梨酸和糖精钠在0.2~20.0μg/mL范围内的质量浓度与对应的峰面积呈良好的线性关系,R2在0.99991~0.99998的范围内,检出限为0.005 g/kg水平,定量限为0.02 g/kg,样品的平均加标回收率为96.9%~98.1%,相对标准偏差为2.2%~2.8%。建立的高效液相色谱同时测定苯甲酸、山梨酸和糖精钠的方法灵敏度较高,操作简便,能够在较短时间内完成检测。适用于食品样品中苯甲酸、山梨酸和糖精钠的定量检测。In order to establish a high performance liquid chromatography method for the simultaneous detection of benzoic acid,sorbic acid and sodium saccharin,in the mobile phase system of methanol+0.02 mol/L ammonium acetate solution,by introducing glacial acetic acid change the pH of the buffer solution,change the gradient elution ratio,and then improve the selectivity of chromatographic peak separation.With ANPU-WP C18(250×4.6 mm,5μm)as separation column,the analysis was performed at the wavelength of 230 nm,the flow rate was set to 1.0 mL/min,and the injection volume was 20μL.Methanol:0.02 mmol/L ammonium acetate solution(pH=6.5)(10︰90,v:v)was used as the mobile phase,and the pH of the buffer solution and the gradient elution procedure of the mobile phase were optimized.Under the optimized chromatographic conditions,the mass concentrations of benzoic acid,sorbic acid and sodium saccharin in the range of 0.2 to 20.0μg/mL showed a good linear relationship with the corresponding peak areas,and R2 in the range of 0.99991~0.99998,the detection limit reached 0.005 g/kg level,and the quantification limit reached 0.02 g/kg level.The average spiked recoveries of the samples were 96.9%~98.1%,and the relative standard deviations were 2.2%~2.8%.The method could be used for the determination of benzoic acid,sorbic acid and saccharin sodium in food samples with with accurate and reliable results.

关 键 词：高效液相色谱法 苯甲酸 山梨酸 糖精钠 食品 

分 类 号：O657.32[理学—分析化学]