用串联质谱法痕量测定 2-氨基吡啶:替诺昔康 api 中一种潜在的基因毒性杂质

Manoj Kumar Rathore, T. Rama, Mohan Reddy, Manoj Kumar
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研究目的本研究旨在采用联用技术,建立一种高灵敏度的方法来测定替诺昔康中的基因毒性杂质 2-氨基吡啶:方法:采用液相色谱-串联质谱(LC-MS/MS)方法,在选择离子监测(SIM)模式下测定 2-氨基吡啶。采用 LiChrospher RP-18 (100×4.6 mm) 5.0 µm 色谱柱进行分离。乙腈(流动相 A)和 0.01M 乙酸铵缓冲液(流动相 B)以不同的比例进行梯度洗脱。梯度程序(T/%B)设定为 0/5、2.50/15、5.00/30、10.00/50、15.00/95、20.00/95。所开发的方法按照国际协调会议的准则进行了验证:2- 氨基吡啶的检出限(LOD)和定量限(LOQ)分别为 0.09 ppm 和 0.3 ppm。该方法的准确度在 89.1%至 106.6%之间。该方法的线性范围为 6 ppm 至 75 ppm,对应于 20 mg/ml 的替诺昔康浓度:本研究中开发的联用 LC-MS/MS 方法可高灵敏、准确地测定替诺昔康中的基因毒性杂质 2-氨基吡啶。该方法的 LOD 值和 LOQ 值均经过验证,准确性也得到了证明,是一种可靠的质量控制工具,适用于定量检测药物化合物替诺昔康中极低浓度的 2-氨基吡啶。
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TANDEM MASS SPECTROMETRIC METHOD FOR THE TRACE LEVEL DETERMINATION OF 2-AMINOPYRIDINE: A POTENTIAL GENOTOXIC IMPURITY IN TENOXICAM API
Objective: This study aimed to develop a highly sensitive method for the determination of the genotoxic impurity 2-amino pyridine in Tenoxicam, employing hyphenated techniques. Methods: The determination of 2-amino pyridine was carried out using a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method in Selected Ion Monitoring mode (SIM). A LiChrospher RP-18 (100×4.6 mm) 5.0 µm column was utilized for the separation. A gradient elution technique was employed with acetonitrile (mobile phase A) and 0.01M ammonium acetate buffer (mobile phase B) in varying ratios. The gradient program (T/%B) was set as 0/5, 2.50/15, 5.00/30, 10.00/50, 15.00/95, 20.00/95. The developed method was validated according to the International Conference on Harmonization guidelines. Results: The limits of detection (LOD) and quantification (LOQ) for 2-amino pyridine were found to be 0.09 ppm and 0.3 ppm, respectively. The method demonstrated accuracy within the range of 89.1% to 106.6% for the analyte. The method's linearity was confirmed through a six-point calibration graph spanning 6 ppm to 75 ppm, corresponding to a concentration of 20 mg/ml of Tenoxicam. Conclusion: Developed hyphenated LC-MS/MS method presented in this study offers a highly sensitive and accurate means for the determination of the genotoxic impurity 2-amino pyridine in Tenoxicam. With validated LOD and LOQ values, as well as demonstrated accuracy, this method proves to be a robust quality control tool suitable for the quantitation of 2-amino pyridine at very low concentrations in the pharmaceutical compound Tenoxicam.
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