超高效液相色谱串联质谱法测定自制奶茶中7种防腐剂和7种甜味剂

Determination of 7 Preservatives and 7 Sweeteners in Homemade Milk Tea Beverages by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry

建立超高效液相色谱-串联质谱法同时测定自制奶茶饮料中的7种甜味剂和7种防腐剂的分析方法。样品经50%甲醇水混合溶液提取后,加入适量沉淀剂沉淀,离心,采用SB-C18色谱柱(50 mm×2.1 mm,1.8μm)分离,以甲醇-水为流动相,梯度洗脱,采用电喷雾负离子模式和多反应监测模式进行检测,外标法定量。结果表明,苯甲酸、山梨酸、脱氢乙酸、糖精钠和对羟基苯甲酸丁酯在5~200 ng·mL^(-1),以及甜蜜素、安赛蜜、三氯蔗糖、纽甜、阿斯巴甜、阿力甜、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯和对羟基苯甲酸丙酯在2~200 ng·mL^(-1)的线性相关系数均>0.995。苯甲酸、山梨酸、脱氢乙酸、糖精钠和对羟基苯甲酸丁酯定量限为0.050 mg·kg^(-1),甜蜜素、安赛蜜、三氯蔗糖、纽甜、阿斯巴甜、阿力甜、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯和对羟基苯甲酸丙酯的定量限为0.020 mg·kg^(-1)。各物质的加标回收率在87.2%~107.6%,相对标准偏差均<10%。该方法简单快速、灵敏度高、重现性好,适用于自制奶茶饮料中14种食品添加剂的快速检测,可满足日常检验工作需要。

An analytical method for the simultaneous determination of 7 sweeteners and 7 preservatives in homemade milk tea beverages by ultra-high performance liquid chromatography-tandem mass spectrometry was established.After the samples were extracted by 50%methanol and water mixed solution,an appropriate amount of precipitant was added to precipitate,centrifuged,and separated by SB-C18 column(50 mm×2.1 mm,1.8μm),methanol-water was used as mobile phase,gradient elution,electrospray anion mode and multiple reaction monitoring mode were used for detection,and external standard method was used for quantification.The results showed that the linear correlation coefficients of benzoic acid,sorbic acid,dehydroacetic acid,sodium saccharin,and butyl p-hydroxybenzoate were all more than 0.995 in the range of 5 ng·mL^(-1)to 200 ng·mL^(-1),and those of cyclamate,acesulfame potassium,sucralose,neotame,aspartame,alitame,methyl p-hydroxybenzoate,ethyl p-hydroxybenzoate,and propyl p-hydroxybenzoate were all more than 0.995 in the range of 2 ng·mL^(-1)to 200 ng·mL^(-1).The limits of quantification of benzoic acid,sorbic acid,dehydroacetic acid,sodium saccharin and butylparaben were 0.050 mg·kg^(-1),and the limits of quantification of cyclamate,acesulfame potassium,sucralose,neotame,aspartame,alitame,methylparaben,ethylparaben and propylparaben were 0.020 mg·kg^(-1).The recovery rate of the spike was 87.2%to 107.6%,and the relative standard deviation was less than 10%.This method is simple,rapid,sensitive and reproducible,and is suitable for the rapid detection of 14 kinds of food additives in homemade milk tea beverages,which can meet the needs of daily inspection work.