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    反相高效液相色谱法同时测定壮阳类保健品中达泊西汀和4种PDE5抑制剂

    Simultaneous Determination of Dapoxetine and 4 PDE5 Inhibitors in Aphrodisiac Health-Care Products by RP-HPLC

    • 摘要: 提出了反相高效液相色谱法同时测定壮阳类保健品中4种PDE5抑制剂和达泊西汀含量的方法。样品溶于水中,再加甲醇提取。分取10 μL提取液进样,并用Inertsil ODS-SP色谱柱为分离柱和由(A)三乙胺-乙酸-水(8+4+988)混合液,(B)乙腈和(C) 0.02%(φ)磷酸溶液三者按不同比例相混的混合液作流动相进行梯度淋洗和分离。在检测波长290 nm处进行测定。他达那非的质量浓度在1.25~25.0 mg·L-1范围内与其峰面积呈线性关系,其余4种化合物的质量浓度在5.0~100 mg·L-1范围内与其峰面积呈线性关系,方法的检出限(3S/N)在0.05~0.2 mg·L-1之间。加标回收率在94.1%~109%之间,测定值的相对标准偏差(n=6)均小于1.0%。

       

      Abstract: A method for simultaneous determination of dapoxetine and 4 PDE5 inhibitors in aphrodisiac health-care products by RP-HPLC was proposed. The sample was dissolved in water and extracted with methanol. The extract (10 μL) was introduced and separated by using Inertsil ODS-SP chromatographic column as stationary phase and mixtures of 0.8% (φ) triethylamine-0.4% (φ) acetic acid,acetonitile and 0.02% (φ) H3PO4 solution with different mixing ratios as mobile phase in the gradient elution. UV-detection at 290 nm was adopted in the determination.Linear relationships between values of peak area and mass concentration of tadalafil was kept in the range of 1.25-25.0 mg·L-1 and for the other 4 compounds in the same range of 5.0-100 mg·L-1. Detection limits (3S/N) found were ranged from 0.05 to 0.2 mg·L-1. Values of recovery found by standard addition method were in the range of 94.1%-109%, with values of RSD′s (n=6) less than 1.0%.

       

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