高效液相色谱法测定食品中山梨酸、苯甲酸、糖精钠的基质干扰分析及定性确证  

Analysis and Qualitative Confirmation of Matrix Interference in the Determination of Sorbic Acid,Benzoic Acid,and Saccharin Sodium in Foods by High Performance Liquid Chromatography

作　　者：丁梅 DING Mei(Meihekou Food and Drug Testing Center,Meihekou 135000,China)

机构地区：[1]梅河口市食品药品检验检测中心,吉林梅河口135000

出　　处：《食品安全导刊》2022年第36期63-67,共5页China Food Safety Magazine

摘　　要：目的:分析食品中山梨酸、苯甲酸、糖精钠测定的基质干扰峰及定性确证。方法:采用高效液相色谱法测定食品中的山梨酸、苯甲酸、糖精钠,当以乙酸铵溶液(20 mmol·L^(-1))+甲醇(95+5)为流动相出现可疑峰时,再以甲酸-乙酸铵溶液(2 mmol·L^(-1)甲酸-20 mmol·L^(-1)乙酸铵)+甲醇(92+8)为流动相分析可疑峰,在两种流动相(不同pH值)洗脱下,比较标液中目标峰与样品中可疑峰保留时间的一致性,定性确认样品中的可疑峰是否为目标峰。结果:基质复杂的样品,单一以一种流动相的保留时间定性,容易出现假阳性情况,而以两种流动相保留时间综合定性验证,才能使样品检测结果更可靠。结论:采用两种流动相洗脱下的保留时间进行综合定性分析,可有效避免样品基质干扰出现假阳性样品。Objective:To analyze the matrix interference peaks in the determination of sorbic acid,benzoic acid and saccharin sodium in foods and to qualitatively confirm them.Method:The sorbic acid,benzoic acid and saccharin sodium in foods were determined by HPLC.When the suspicious peak appeared in the mobile phase of ammonium acetate solution(20 mmol·L^(-1))+methanol(95+5),and then the mobile phase of formic acid-ammonium acetate solution(2 mmol·L^(-1)formic acid-20 mmol·L^(-1)ammonium acetate)+methanol(92+8)was used to analyze the suspicious peak.Compare the consistency of retention time between the target peak in the standard solution and the suspicious peak in the sample,and qualitatively confirm whether the suspicious peak in the sample is the target peak.Result:For samples with complex matrix,the retention time of one mobile phase alone can easily lead to false positive.However,the comprehensive qualitative verification of the retention time of two mobile phases can make the sample test results more reliable.Conclusion:Using the retention time under the elution of two mobile phases for comprehensive qualitative analysis can effectively avoid the false positive sample caused by sample matrix interference.

关 键 词：高效液相色谱法 山梨酸 苯甲酸 糖精钠 基质干扰峰 定性确证 

分 类 号：O657.72[理学—分析化学] TS207.3[理学—化学]