超高效液相色谱-串联质谱法同时测定食醋、酱油及料酒中的13种甜味剂和防腐剂

Simultaneous determination of 13 preservatives and sweeteners in vinegar, soy sauce and seasoning wine by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  食醋  酱油  料酒  甜味剂  防腐剂

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  vinegar  soy sauce  seasoning wine  sweetener  preservatives

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定食醋、酱油及料酒中13种甜味剂和防腐剂含量的分析方法。方法 采用Atlantis? T3色谱柱(2.1 mm×150 mm, 3 μm), 柱温30 ℃, 流动相由A(甲醇)和B(10 mmol/L甲酸和10 mmol/L甲酸铵溶液)组成, 梯度洗脱, 流速0.2 mL/min。采用电喷雾负离子(electron spray ionization, ESI-)模式电离, 多反应监测(multiple reaction monitoring, MRM)模式检测, 外标法定量。结果 此方法可快速准确检测苯甲酸等13种甜味剂和防腐剂, 浓度范围在1~200 mg/kg内线性相关良好, 相关系数(r)均大于0.996, 平均回收率为85.7%~112.1%, 相对标准偏差(relative standard deviation, RSD)为2.2%~7.7% (n=6)。结论 该方法快速、准确, 灵敏度高, 适用于食醋、酱油及料酒中13种甜味剂和防腐剂的快速筛查和定量分析。

英文摘要:

      Objective To establish a method for simultaneous determination of 13 preservatives and sweeteners in vinegar, soy sauce and seasoning wine by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods The chromatographic separations were obtained on a Atlantis? T3 column (2.1 mm× 150 mm, 3 μm) using the phase A (methanol), and mobile phase B (10 mmol/L formic acid and 10 mmol/L ammonium formate in water) as mobile phase. The flow rate was 0.2 mL/min for gradient elution, and the column temperature was held at 30 ℃. Under the electro spray ionization (ESI-) mode with negative ions, multiple reactions monitoring (MRM) was used as the basis for quantitative analysis by external standard method. Results This method could quickly and accurately detect preservatives and sweeteners, such as benzoic acid. The 13 preservatives and sweeteners had good linear relationships in the range of 1?200 mg/kg, and the correlation coefficients (r) were all more than 0.996. The average recoveries were 85.7%?112.1%, with relative standard deviation (RSD) of 2.2%?7.7% (n=6). Conclusions This method is rapid, accurate and sensitive, and is suitable for the rapid screening and quantitative analysis of 13 preservatives and sweeteners in vinegar, soy sauce and seasoning wine.