摘要
目的:建立了超高效液相色谱-串联质谱法测定食用农产品(水果)中14种甜味剂的分析方法。方法:水果样品经50%(V/V)甲醇水溶液提取后,萃取液经HLB(Hydrophilic lipophilic balance)固相萃取柱净化和氮吹浓缩,采用Acquity UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm)进行分离,以甲醇-10 mmol/L乙酸铵水溶液为流动相进行梯度洗脱,柱温35℃,流速为0.35 mL/min,利用电喷雾离子源多反应监测模式对14种甜味剂进行定性离子、定量检测。结果:14种甜味剂在相应的浓度范围内线性关系良好(R2≥0.994),方法检出限在0.09~1.65μg/L之间,定量限在0.17~4.89μg/L之间。3个不同加标浓度水平的回收率在84.7%~107.5%之间,相对标准偏差(n=6)在3.2%~8.5%之间。结论:该方法样品前处理简单、重现性好、灵敏度高、准确度高,可适用于食用农产品(水果)中14种甜味剂的同时测定。
Objective:To establish a method for simultaneous determination of 14 sweeteners in edible agricultural products(fruits)by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods:The fruit samples were extracted by 50%(V/V)methanol solution,the extract was purified by HLB solid phase extraction column and concentrated by nitrogen blowing,the separation was achieved using an Acquity UPLC HSS T_3 column(2.1 mm×100 mm,1.8μm)with a methanol-10 mmol/L ammonium acetate aqueous solution gradient elution,the column temperature was set at 35°C with a flow rate of 0.35 mL/min,the detection and quantification were performed using electrospray ionization multiple reaction monitoring mode for 14 sweeteners.Results:The calibration curves for the 14 sweeteners showed good linearity within their respective concentration ranges(R~2≥0.994).The limits of detection(LODs)and the limits of quantification(LOQs)ranged from 0.09μg/L to 1.65μg/L and 0.17μg/L to 4.89μg/L,the average recoveries varied from 84.7%to 107.5%at three different levels,and the relative standard deviations(RSDs)ranged from 3.2%to 8.5%(n=6).Conclusion:This method has the advantages of simple sample pretreatment,good reproducibility,high sensitivity and high accuracy,and can be applied to the simultaneous determination of 14 kinds of sweeteners in edible agricultural products(fruits).
作者
钟永生
万承波
朱钦
程丽美
章明
管鹏
黄磊
ZHONG Yongsheng;WAN Chengbo;ZHU Qin;CHENG Limei;ZHANG Ming;GUAN Peng;HUANG Lei(Jiangxi General Institute Testing and Certification Industry Product Testing Institute,Nanchang330029,China)
出处
《食品科技》
CAS
北大核心
2024年第4期315-321,共7页
Food Science and Technology
基金
江西省市场监督管理局科技项目(GSJK202119)。
关键词
超高效液相色谱-串联质谱
甜味剂
食用农产品
水果
同时测定
ultra performance liquid chromatography-tandem mass spectrometry
sweeteners
edible agricultural products
fruits
simultaneous determination
作者简介
钟永生(1988-),男,江西南昌人,硕士,工程师,研究方向为化学检测与分析。
