超高效液相色谱-串联质谱法同时测定食品中7种防腐剂和4种甜味剂

Simultaneous determination of 7 kinds of preservatives and 4 kinds of sweeteners in foods by UPLC-MS/MS

目的:建立一种超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定食品中7种防腐剂(苯甲酸、山梨酸、脱氢乙酸、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯)和4种甜味剂(糖精钠、甜蜜素、安赛蜜、三氯蔗糖)。方法:样品经提取液提取(乙醇∶水=8∶2,体积比),用2.5mL乙酸锌和2.5mL亚铁氰化钾沉淀蛋白,加提取液定容至刻度,漩涡震荡10min,离心,取上清液进行测定。结果:本方法线性关系良好(r^2=0.9921~0.9995),检出限为0.5μg/kg^10μg/kg。在不同食品中3个浓度添加水平平均回收率为79.5%~107.1%,相对标准偏差为0.7%~6.5%。结论:该方法准确度高,结果稳定可靠,适用于食品中多种防腐剂和甜味剂的高通量检测。

Objective ：To establish a Ultra performance liquid chromatography tandem mass spectrometry method（UPLC-MS/MS）for simultaneous determination of 7 kinds of preservatives（benzoic acid,sorbic acid,dehydroacetic acid,methylparaben,ethylparpben,eropylparaben,butylparaben）and 4 kinds of sweeteners（saccharin sodium,sodium N-cyclohexylsulfamate,acesulfame potassium,sucralose）. Method ： The samples were extracted with extraction solution（ethanol ∶ water=8 ∶ 2,v/v）, precipatated protein by 2.5mL zinc acetate and 2.5m L potassium ferrocyanide,diluted with extraction solution to volume,carried on a vortex shock for 10 minutes,centrifugated and the supernatant was got for future determination.Result ：The method showed good linearity（r^2=0.9921 ~ 0.9995）,the detection limits were 0.5μg/kg ~ 10μg/kg.The average recoveries of three levels in different foods is 79.5% ~ 107.1% and the RSDs were 79.5% ~ 107.1%.Conclusion ：The method has a high accuracy, the result is stable and reliable, and suitable for the high-throughput determination of multiple kinds of preservatives and sweeteners in foods.