超高效液相色谱-串联质谱法测定酒类产品中13种添加剂

Simultaneous Determination of 13 Food Additives in Alcoholic Drinks by UPLC-MS/MS

建立超高效液相色谱-串联质谱(ultra high performance liquid chromatography tandem mass spectrometry,UPLC-MS/MS)同时测定酒类产品中13种食品添加剂含量的分析方法。采用Agilent EC-C_(18)色谱柱(4.6 mm×50 mm,2.7μm),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(ESI-)模式电离,多反应监测(multiple reaction monitoring,MRM)模式检测,外标法定量。结果表明,在最佳条件下,13种食品添加剂可在10 min内有效分离,标准曲线线性关系良好(r>0.998)。平均回收率为88.7%~107.1%,相对标准偏差为2.2%~8.7%,检出限为0.02~0.26 mg/kg,平均加样回收率89.9%~104.2%。该方法快速、准确,灵敏度高,适用于酒类产品中甜味剂、防腐剂等13种食品添加剂的快速筛查和定量分析。

In this study we established a method for the simultaneous determination of 13 food additives in alcoholic drinks by UPLCMS/MS.The chromatographic separations were obtained on an Agilent EC-C_(18) column(4.6 mm×50 mm,2.7μm)at 30℃.Gradient elution was carried out with methanol as phase A and 10 mmol/L formic acid and 10 mmol/L ammonium formate solution as phase B,and the flow rate was 0.2 mL/min.Electrospray ionization in negative ion mode(ESI-)and multiple reactions monitoring(MRM)were adopted as the basis for quantitative analysis by external standard method.Under the optimal conditions,the 13 food additives could be effectively separated within 10 min.The standard curves had good linearity(r>0.998).The average recoveries were in the range of 88.7%to 107.1%,the relative standard deviations(RSDs)were 2.2%to 8.7%,the limits of detection(LODs)were 0.02 mg/kg to 0.26 mg/kg,and the average spiked recoveries were 89.9%to 104.2%.The method is rapid,accurate and sensitive,and is suitable for the rapid screening and quantitative analysis of the 13 food additives in alcoholic drinks,including sweeteners and preservatives.