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    超高效液相色谱-串联质谱法测定壮阳类保健品中非法添加的5种5型磷酸二酯酶抑制剂

    UPLC-MS/MS Determination of 5 Kinds of Phosphodiesterase Type 5 Inhibitors Illegally Added in Aphrodisiac Health Products

    • 摘要: 称取经研磨后的样品0.500 0 g,用甲醇超声溶解,并定容至50 mL,以10 000 r·min-1转速离心10 min,上清液经0.25 μm滤膜过滤后,采用Waters Symmetry Shield RP色谱柱(100 mm×2.1 mm,5 μm)分离5种5型磷酸二酯酶(PDE-5)抑制剂(西地那非、他达拉非、红地那非、伐地那非、伪伐地那非),以含0.1%(体积分数,下同)甲酸的甲醇和含0.1%甲酸的10 mmol·L-1乙酸铵溶液为流动相,进行梯度洗脱。在电喷雾正离子模式下以多反应监测模式检测,采用外标法定量。结果表明,5种PDE-5药物的质量浓度在一定范围内与其峰面积呈线性关系,检出限(3S/N)为0.25~0.43 mg·kg-1。加标回收率为97.2%~104%,测定值的相对标准偏差(n=6)为0.31%~1.1%。方法用于检测62种壮阳类保健品中上述5种PDE-5药物,共有37种保健品中检出非法添加药物。

       

      Abstract: The grinded sample (0.500 0 g) was ultrasonically dissolved with methanol, and the solution was diluted to 50 mL with methanol and centrifuged at 10 000 r·min-1 for 10 min. After the supernatant was filtrated with 0.25 μm filter membrane, 5 kinds of illegally added phosphodiesterase type 5 inhibitors (PDE-5) (sildenafil, tadalafil, acetildenafil, vardenafil, pseudo-vardenafil) were separated on a Waters Symmetry Shield RP column (100 mm×2.1 mm, 5 μm), with methanol containing 0.1% (φ) formic acid and 10 mmol·L-1 ammonium acetate solution containing 0.1% formic acid as the mobile phase for gradient elution. The determination was conducted in positive ESI mode under multiple reaction monitoring mode, with external standard method for quantification. Linear relationships were found between peak areas and mass concentrations of 5 kinds of PDE-5 medicines in definite ranges, with detection limits (3S/N) in the range of 0.25-0.43 mg·kg-1. Values of recovery obtained by standard addition method were in the range of 97.2%-104%, and RSDs (n=6) ranged from 0.31% to 1.1%. The method was applied to determination of the above PDE-5 medicines in 62 kinds of aphrodisiac health products, and the results showed that 37 kinds of aphrodisiac health products contained illegal added medicines.

       

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