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    超高效液相色谱-串联质谱法测定减肥类保健品中的西布曲明

    Determination of Sibutramine in Weight-Loss by UHPLC-MS/MS

    • 摘要: 采用超高效液相色谱-串联质谱法测定减肥类保健品中的西布曲明.样品经甲醇超声提取后,使用Phenomenex Kinetex C18色谱柱分离,以乙腈-10 mmol·L-1乙酸铵溶液(含0.1%甲酸)为流动相进行梯度洗脱,质谱中选择多反应选择离子监测模式检测,以西布曲明-D6作为同位素内标进行定量.西布曲明的质量浓度在5.00~400 μg·L-1范围内呈线性,测定下限(10S/N)为10 ng·g-1.加标回收率在97.0%~104%之间,相对标准偏差(n=9)为1.1%~3.0%.

       

      Abstract: UHPLC-MS/MS was used for the determination of sibutramine in health products for weight-loss. The sample was extracted with methanol by ultrasonic,then separated on a Phenomenex Kinetex C18 column with the mixture of acetonitrile and 10 mmol·L-1 ammonium acetate solution containing 0.1% (φ) formic acid solution as mobile phase for gradient elution. MRM was adopted in MS detection. D6-Sibutramine was used as internal standard for quantification. The linear range for the mass concentration of sibutramine was 5.00-400 μg·L-1,and the lower limit of determination (10S/N) was 10 ng·g-1. The recovery rates measured by standard addition method were in the range of 97.0%-104%,with RSD (n=9) in the range of 1.1%-3.0%.

       

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