高效液相色谱-串联质谱法快速测定清咽润喉类食品中13种非法添加药物含量

Rapid determination of 13 kinds of illegally added drugs in throat clearing and moistening foods by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  清咽润喉  食品  保健食品  非法添加  高效液相色谱-串联质谱

英文关键词:throat clearing and moistening  health food  illegal addition  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定清咽润喉类食品中13种非法添加药物含量的方法。方法 针对清咽润喉类食品中4种常见的食品类型, 样品使用70%甲醇水溶液进行超声提取和定容, 经Waters ACQUITY UPLC?HSS T3 (2.1 mm×100 mm, 1.8 μm)分离, 流动相为5 mmol/L乙酸铵-0.1%甲酸水溶液和甲醇, 洗脱方式为梯度洗脱。在电喷雾正离子模式下, 采用多反应监测(multiple reaction monitoring, MRM)模式检测, 使用基质标准曲线进行定量。结果 13种化合物得到较好分离, 在一定范围内线性关系良好(r2>0.99)。待测化合物中, 12种化合物较为稳定, 头孢氨苄容易降解, 根据稳定性实验结果显示, 13种化合物在18 h内相对标准偏差(relative standard deviations, RSDs)值小于等于18.00%。在阴性样品中分别添加低、中、高3个浓度水平的13种化合物, 13种化合物的回收率满足60%~120%, RSDs值均小于20.00%, 满足分析要求。结论 经方法学验证, 该方法简便、准确, 可用于4种类型的清咽润喉类食品中13种非法添加物的测定。

英文摘要:

      Objective To establish a method for the determination of 13 kinds of illegally added drugs in throat clearing and moistening foods by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods For the 4 common kinds of throat clearing and moistening foods, samples were extracted and made up to volume with 70% methanol water solution by ultrasonic extraction. The separation was carried out on a Waters ACQUITY UPLC?HSS T3 column (2.1 mm×100 mm, 1.8 μm), with the mobile phase consisting of 5 mmol/L ammonium acetate-0.1% formic acid aqueous solution and methanol, and the elution mode was gradient elution. Detection was performed in the positive ion mode of electrospray ionization using the multiple reaction monitoring (MRM) mode, and quantification was carried out using a matrix standard curve. Results The 13 kinds of compounds were well separated, and showed good linear relationships within a certain range (r2>0.99). Among the compounds to be tested, 12 kinds of compounds were relatively stable, while cephalexin was prone to degradation. According to the stability experiment results, the relative standard deviations (RSDs) of the 13 kinds of compounds were less than or equal to 18.00% within 18 hours. In the negative samples, 13 kinds of compounds at 3 different concentration levels (low, medium and high) were added respectively. The recovery rates of the 13 kinds of compounds ranged from 60% to 120%. The RSDs were all less than 20.00%, meeting the analytical requirements. Conclusion After methodological validation, this method is simple, accurate, and can be used for the determination of 13 kinds of illegally added substances in 4 kinds of throat clearing and moistening foods.