LC-AJS ESI-MS/MS同时测定果露酒中7种甜味剂、2种防腐剂和柠檬酸

Determination of 7 Sweeteners,2 Preservatives and Citric Acid in Fruit Wineby LC-AJS ESI-MS/MS

利用液相质谱联用仪(AJS ESI离子源),对果露酒中的安赛蜜、糖精钠、甜蜜素、三氯蔗糖、阿斯巴甜、纽甜、阿力甜7种甜味剂,苯甲酸、山梨酸2种防腐剂,以及柠檬酸进行同时检测。对于澄清透明的样品,采用加水稀释,超声混匀方式进行前处理;对于浑浊度较高的,采用加入亚铁氰化钾和乙酸锌溶液进行沉淀,取上清液过0.22μm滤膜上机检测。采用Agilent SB-C_(18) RRHD(2.1 mm×50 mm,1.8μm)作为分析柱,以0.1%乙酸-5 mmol/L乙酸铵和甲醇作为流动相进行梯度洗脱,在电喷雾正/负离子模式下,利用多反应监测模式(MRM)进行分析检测。结果表明:方法检出限为5~10μg/kg,定量限为10~20μg/kg;线性范围为1.00×10^(-3)~1.0 mg/L,线性线性相关系数均大于0.99;重复性和再现性相对偏差1.2%~7.6%(n=6);加标浓度范围为1.00×10^(-4)~5.00×10^(-3) g/kg,加标回收率在88.4%~110%之间。试验方法前处理步骤少且易于操作,经过前处理后的样品基质干扰小,目标物检测灵敏度高,适用于果露酒中7种甜味剂、2种防腐剂和柠檬酸的快速检测。

The method uses a liquid phase mass spectrometer(AJS ESI Ion Source)for the 7 sweeteners of acesulfame,sodium saccharin,cyclamate,sucralose,aspartame,neotame and alitame,2 preservatives of benzoic acid and sorbic acid,and citric acid.For clear and transparent samples,pre-treatment with water dilution and ultrasonic mixing,and precipitation with potassium ferrocyanide and zinc acetate solutions for high turbidity samples,the supernatant was detected by 0.22μm filter membrane.Agilent SB-C_(18) RRHD(2.1 mmx50 mm,1.8μm)was used as the analytical column;0.1%acetic acid-5 mmol/L ammonium acetate and methanol were used as the mobile phase for gradient elution;Multi-reaction monitoring mode(MRM)was used for analysis and detection.The results showed that the detection limit was 5-10μg/kg;The quantitative limit was 10-20μg/kg;The linear range was 1.00x10^(-3)-1.0 mg/L;The linear correlation coefficient was more than 0.99;The relative deviation of reproducibility and reproducibility was 1.2%-7.6%(n=6).The range of standard concentration was 1.00x10^(-4)-5.00x10^(-3)g/kg,and the recovery was 88.4%-110%.The method had the advantages of less steps of pretreatment,less matrix interference and high sensitivity,and it was suitable for rapid detection of 7 sweeteners,2 preservatives and citric acid in fruitwine.