Dapoxetine hydrochloride is a selective serotonin reuptake inhibitor drug for treating premature ejaculation. This study was designed to develop and validate a sensitive and selective LC–MS/MS method for trace analysis of genotoxic impurity ethyl methanesulfonate in Dapoxetine hydrochloride. Chromatographic separation was achieved on the Shodex RSpak DS-413 column, 150 × 4.6 mm, 3.0 µm using eluent containing a equal volumes of acetonitrile and 0.1% v/v formic acid in water was used in the isocratic elution mode at a pump flow of 1.0 mL/min. No interference was observed at the retention time of ethyl methanesulfonate, indicating that the developed method is specific and selective for trace level quantification.The developed method was found to be linear in the concentration range of 1–50 ppm with coefficient of regression of 0.9997. Detection limit and quantification limit were determined to be 0.6 ppm and 1.0 ppm respectively. Acceptable RSD values (< 10.0%) and recovery results (> 90%) obtained from the accuracy and precison experiments indicate that the developed method is precise and accurate in the concentration range of 1–50 ppm. Ethyl methanesulfonate solutions were stable for two days when stored at room and refrigerated temperatures. The developed method has the ability to quantify ethyl methanesulfonate in dapoxetine hydrochloride. Thus, the anticipated method has high probability to adopt in the quality testing laboratories of pharmaceutical industry.

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液相色谱-串联质谱法对甲磺酸乙酯进行痕量定量：盐酸达泊西汀中的遗传毒性杂质

盐酸达泊西汀是一种选择性血清素再摄取抑制剂，用于治疗早泄。本研究旨在开发和验证一种灵敏且选择性的 LC-MS/MS 方法，用于对盐酸达泊西汀中的遗传毒性杂质甲磺酸乙酯进行痕量分析。在 Shodex RSpak DS-413 色谱柱上实现色谱分离，150 × 4.6 mm，3.0 µm，使用含有等体积乙腈和 0.1% v/v 甲酸水溶液的洗脱液，在等度洗脱模式下，泵流量为1.0 毫升/分钟。在甲磺酸乙酯的保留时间未观察到干扰，表明所开发的方法对痕量水平的定量具有特异性和选择性。发现所开发的方法在 1-50 ppm 的浓度范围内呈线性，回归系数为 0.9997。检测限和定量限分别确定为 0.6 ppm 和 1.0 ppm。从准确度和精密度实验中获得的可接受的 RSD 值 (< 10.0%) 和回收率结果 (> 90%) 表明，所开发的方法在 1–50 ppm 的浓度范围内是精密准确的。甲磺酸乙酯溶液在室温和冷藏温度下可稳定保存两天。所开发的方法能够量化达泊西汀盐酸盐中的甲磺酸乙酯。因此，预期的方法很有可能被制药行业的质量检测实验室采用。90%) 从准确度和精密度实验中获得的结果表明，所开发的方法在 1-50 ppm 的浓度范围内是精密和准确的。甲磺酸乙酯溶液在室温和冷藏温度下可稳定保存两天。所开发的方法能够量化达泊西汀盐酸盐中的甲磺酸乙酯。因此，预期的方法很有可能被制药行业的质量检测实验室采用。90%) 从准确度和精密度实验中获得的结果表明，所开发的方法在 1-50 ppm 的浓度范围内是精密和准确的。甲磺酸乙酯溶液在室温和冷藏温度下可稳定保存两天。所开发的方法能够量化达泊西汀盐酸盐中的甲磺酸乙酯。因此，预期的方法很有可能被制药行业的质量检测实验室采用。