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作 者:淳泽利 谷莹莹 陈荣祥 CHUN Zeli;GU Yingying;CHEN Rongxiang(Life Sciences Institute,Zunyi Medical University,Zunyi 563000,China;Zunyi Engineering Technology Research Center of Physical and Chemical Analysis,Zunyi Medical University,Zunyi 563000,China;School of Public Health,Zunyi Medical University,Zunyi 563000,China)
机构地区:[1]遵义医科大学生命科学研究院,遵义563000 [2]遵义医科大学遵义市理化分析测试工程技术研究中心,遵义563000 [3]遵义医科大学公共卫生学院,遵义563000
出 处:《理化检验(化学分册)》2022年第6期670-676,共7页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:国家自然科学基金项目(81760652);遵义医科大学硕士启动资金项目(F-972);遵义市汇川区科技计划项目(遵汇科合201827)。
摘 要:取10 g饮料样品,加水稀释并定容至50 mL,混合均匀,取少量混合液以转速10000 r·min^(-1)离心10 min,上清液经0.22μm滤膜过滤后,以ACQUITY UPLC~?BEH C_(18)色谱柱为固定相,电化学检测器(ECD)检测,检测池电压为650 mV,采用超高效液相色谱法测定其中爱德万甜、根皮苷、柚皮苷二氢查耳酮、三叶苷、新橙皮苷二氢查耳酮、根皮素的含量。结果表明,爱德万甜和5种二氢查耳酮类甜味剂在9.0 min内可以完全分离,其质量浓度在一定范围内与其对应的峰面积呈线性关系,检出限(3S/N)为2.1~6.8μg·L^(-1)。按标准加入法进行回收试验,回收率为97.1%~105%,测定值的相对标准偏差(n=6)为1.4%~5.1%。与二极管阵列检测器(DAD)比较,使用ECD时,灵敏度高、检出限低。与其他文献方法相比,本方法的灵敏度、分析时间均具有明显优势。The drink sample(10 g)was taken,diluted with water and made its volume up to 50 mL.After fully mixing,a small amount of solution was taken and centrifuged for 10 min at a rotating speed of 10000 r·min^(-1).Then the supernatant was filtered by 0.22μm filtration membrane,and advantame,phlorizin,naringin dihydrochalcone,trilobatin,neohesperidin dihydrochalcone and phloretin in the above solution were determined by ultra-high performance liquid chromatography(UHPLC),using ACQUITY UPLC■BEH C_(18) column as the stationary phase,and electrochemical detector(ECD)with the detection cell voltage set at 650 mV.As shown by the results,advantame and 5 sweeteners of dihydrochalcones could be separeted completely within 9.0 min,and linear relationships between values of peak area and mass concentration of advantame and 5 sweeteners of dihydrochalcones were found in definite ranges,with detection limits(3 S/N)ranged from 2.1μg·L^(-1)to 6.8μg·L^(-1).Test for recovery was made by standard addition method,giving results in the range of 97.1%^(-1)05%,with RSDs(n=6)of the determined values in the range of 1.4%-5.1%.Compared with diode array detector(DAD),ECD had higher sensitivity and lower detection limit.Compared with other methods in the literature,this method had obvious advantages of sensitivity and analysis time.
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