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    QuEChERS净化-超高效液相色谱-串联质谱法测定复合调味料中的爱德万甜含量

    UHPLC-MS/MS Determination of Advantame in Compound Seasoning with Purification by QuEChERS

    • 摘要: 称取复合调味料样品1.000 0 g,用甲醇-水(50+50)溶液作为提取剂将样品中爱德万甜溶于提取剂中。先后提取2次,每次加提取剂10 mL,振荡提取10 min,高速离心5 min。收集2次上清液,合并并用水定容至25.0 mL。分取此溶液1.0 mL加入于已装有C18 200 mg和N-丙基乙二胺(PSA)100 mg的EP管中,涡旋混匀1 min,高速离心2 min,取上清液经0.22 μm滤膜过滤。分取滤液5 μL进样,以Agilent ZORBAX SB-C18色谱柱作为固定相,以不同比例的0.1%(体积分数)甲酸溶液(A)和甲醇(B)的混合液作为流动相,按程序进行梯度洗脱。串联质谱分析中采用电喷雾离子源正离子扫描和多反应监测模式。测得爱德万甜的线性范围在0.2~20 μg·L-1之间,其检出限(3S/N)为2.0 μg·kg-1。以调味粉和调味酱样品作为基体,用标准加入法进行回收和精密度试验,测得回收率在89.3%~98.5%之间,测定值的相对标准偏差(n=6)在1.8%~3.8%之间。

       

      Abstract: A portion (1.000 0 g) of compound seasoning sample was extracted twice with mixed solvent of CH3OH and H2O (50+50) to transfer the analyte, advantame, from the sample into solution. 10 mL of the mixed solvent was used in each extraction, which was performed by swirling for 10 min and centrifuging for 5 min with high speed. Supernatants from the 2 extractions were collected and diluted to 25.0 mL with water. An aliquot of 1.0 mL of the solution was mixed by swirling for 1 min with 200 mg of C18 and 100 mg of PSA in an EP tube and centrifuged for 2 min with high speed for purification. The supernatant was filtered through 0.22 μm filtering membrane and 5 μL of the filtrate was introduced into the instrument by using Agilent ZORBAX SB-C18 column as stationary phase and using mixtures of 0.1% (φ) formic acid solution (A) and CH3OH (B) mixed in various rations as mobile phases in the programed gradient elution. ESI with positive ion scanning mode and mode of MRM were adopted in MS/MS. Linearity range for advantame was found between 0.2 to 20 μg·L-1, with detection limit (3S/N) of 2.0 μg·kg-1. Using powdery and pasty seasoning samples as matrixes, tests for recovery and precision were made by standard addition method, giving values of recovery in the range of 89.3% to 98.5%, and values of RSDs (n=6) in the range of 1.8% to 3.8%.

       

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