Simultaneous determination of acetyl vardenafil, homosildenafil, hydroxy acetildenafil and mirodenafil by CE-C4D

Lan Anh Hoang Thi, Oanh Nguyen Thi, Diu Dinh Thi, Nhi Do Yen, Bach Pham Gia, Trang Vu Thi, Anh Huong Nguyen Thi, Hong Hao Le Thi
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Abstract

Dietary supplements are currently popular because of their natural origin, especially male enhancement products. However, some of these products have been found to contain erectile dysfunction drugs that inhibit the enzyme phosphodiesterase-5 (PDE-5), leading to adverse effects on human health. In this study, capillary electrophoresis with capacitively coupled contactless conductivity detection (CE-C4D) was used to determine four PDE-5 inhibitors (including acetyl vardenafil, homosildenafil, hydroxy acetildenafil and mirodenafil) in dietary supplement samples. The optimum analytical conditions included electrolyte solution of 20 mM arginine (Arg)/acetic acid (Ace)/acetonitrile (ACN) 20% pH 6.5, silica capillary 50 μm inner diameter with effective length of 50 cm, separation voltage of 20kV, siphoning hydrodynamic injection at a height of 25 cm for 30 s. At the optimum analytical conditions, the limits of detection of acetyl vardenafil, homosildenafil, hydroxy acetildenafil, and mirodenafil were 2.1, 1.6, 2.3, and 1.3 mg/L, respectively. The analysis of four PDE-5 inhibitors by CE-C4D also showed good repeatability (< 5 %) and recovery (> 97 %). This method was further applied to simultaneously determine the amount of acetyl vardenafil, homosildenafil, hydroxy acetildenafil, and mirodenafil in three functional products. All four PDE-5 inhibitors were not detected in these samples. To demonstrate the utility of this method, the mixture of four PDE-5 inhibitors standard solutions was added to three samples. The recovery was between 98.8 % and 100.6%, illustrating the potential applicability of the method of determining PDE-5 inhibitors in dietary supplement samples.
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CE-C4D法同时测定乙酰伐地那非、异西地那非、羟基伐地那非和咪洛地那非的含量
膳食补充剂目前很受欢迎,因为它们的天然来源,尤其是男性增强产品。然而,其中一些产品被发现含有抑制磷酸二酯酶-5 (PDE-5)酶的勃起功能障碍药物,导致对人体健康产生不利影响。本研究采用毛细管电泳-电容偶联无接触电导率检测法(CE-C4D)检测膳食补充剂样品中的4种PDE-5抑制剂(乙酰基伐地那非、同源西地那非、羟基乙酰地那非和米罗地那非)。最佳分析条件为:电解液为20 mM精氨酸(Arg)/乙酸(Ace)/乙腈(ACN) 20%, pH为6.5,硅胶毛细管内径为50 μm,有效长度为50 cm,分离电压为20kV,虹吸进样高度为25 cm,进样时间为30 s。在最佳分析条件下,乙酰伐地那非、异西地那非、羟基伐地那非和米罗地那非的检出限分别为2.1、1.6、2.3和1.3 mg/L。CE-C4D分析4种PDE-5抑制剂也显示出良好的重复性(< 5%)和回收率(> 97%)。进一步应用该方法同时测定了三种功能产品中乙酰伐地那非、同型西地那非、羟基乙酰伐地那非、美洛地那非的含量。在这些样品中未检测到所有四种PDE-5抑制剂。为了证明该方法的实用性,将四种PDE-5抑制剂标准溶液的混合物加入到三个样品中。回收率在98.8% ~ 100.6%之间,说明了该方法在膳食补充剂样品中测定PDE-5抑制剂的潜在适用性。
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