高效液相色谱-串联质谱法同时测定葡萄酒中甜味剂、防腐剂和色素

Simultaneous Determination of Sweeteners, Preservatives and Pigments in Grape Wine by HPLC-MS/MS

建立了高效液相色谱-串联质谱仪(HPLC-MS/MS)同时测定葡萄酒中甜味剂(安赛蜜、糖精钠、甜蜜素、阿斯巴甜、三氯蔗糖、纽甜、阿力甜和甜菊糖苷)、防腐剂(脱氢乙酸)和色素(诱惑红、赤藓红、苋菜红、胭脂红、柠檬黄、日落黄、亮蓝)含量的新方法。样品经超纯水稀释5倍,微孔滤膜过滤后直接进样,用HPLC-MS/MS进行定量分析。Acquity UPLC HSS T_3柱为分析柱,甲醇-10 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,采用电喷雾离子源(ESI)正负离子切换多反应监测模式(MRM)检测,外标法定量。结果表明,16种添加剂在相应的浓度范围内线性关系良好(相关系数r^2>0.995),方法检出限在0.2～3μg/L之间,在3个不同浓度的添加水平下,平均回收率为89.1%～106.4%,相对标准偏差≤9.7%,满足日常检测的要求。该方法前处理简单,测定快速、准确、灵敏度高,适用于葡萄酒中16种添加剂的快速筛查和定量分析。

A method for simultaneous determination of sweeteners(acesulfame potassium,sodium saccharin,sodium cyclamate,aspartame,sucralose,neotame,alitame and stevioside),preservatives(dehydroacetic acid),and pigments(allura red,erythrosine,amaranth,carmine,lemon yellow,sunset yellow,brilliant blue)had been developed.Wine samples were diluted with distilled water(five times of wine volume),then filtered through 0.22μm microporous membrane,and quantitative analysis was done by HPLC-MS/MS through direct sample injection.LC separation was performed on Shimadzu LC-20ADXR system with a T3 column,acetic acid ammonium(10 mmol/L)and methanol was used as the mobile phase for gradient elution.After LC separation,MS/MS was adopted for multiple reaction monitoring(MRM)in the positive and negative mode.The correlation coefficients of linear calibration curves were higher than 0.995 in the corresponding concentration ranges.The limits of detection(LODs)were between 0.2μg/L to 3μg/L.The average recoveries of the 16 additives ranged from 89.1%to 106.4%,and the relative standard deviations(RSD)were lower than 9.7%in spiked sample at three levels.The results indicated that this method was easier,faster,more sensitive,and suitable for qualitative and quantitative analysis of preservatives,sweeteners and pigments in wine.