Stability-indicating reversed-phase high-performance liquid chromatography (RP-HPLC) and normal-phase high-performance thin-layer chromatography (NP-HPTLC) methods have been developed for the determination of palonosetron which is a potent antiemetic drug used with chemotherapy. Forced degradation studies were performed on palonosetron to study its stability behavior. The drug was subjected to acid, base, neutral hydrolysis, oxidation, thermal and photolytic conditions. Mass analysis has been performed to elucidate the oxidative degradants by Advion compact mass spectrometer. HPLC separation was achieved on PerfectChrom 100 C4 (250 × 4.6 mm, 5 μm particle size) column using buffer (20 mM dipotassium hydrogen orthophosphate, adjusted with phosphoric acid to pH 2.5):acetonitrile:methanol (60:30:10, v/v) as the mobile phase with isocratic mode at a flow rate of 1 mL/min using photodiode array detector (PAD) at 210 nm. The method showed adequate sensitivity concerning linearity, accuracy and precision over the range of 0.1–10 μg/mL. Limit of detection (LOD) and limit of quantification (LOQ) were determined to be 0.03 μg/mL and 0.09 μg/mL, respectively. HPTLC separation was carried out on aluminum plates pre-coated with silica gel 60 F₂₅₄ using methanol:ammonia (10:0.5, v/v) as the mobile phase. CAMAG scanner was operated at 254 nm for the densitometric measurement in the absorbance mode. A polynomial relationship was constructed in concentration range of 0.1–2 μg/band, with LOD and LOQ 0.02 μg/band and 0.06 μg/band, respectively. The cited chromatographic methods were successfully applied to the determination of palonosetron in the presence of its degradation products and additives in the commercially available vials. Method validation was performed as per the ICH guidelines confirming methods robustness to be used in quality control laboratories. Statistical comparisons have been performed between the results of the cited chromatographic methods and those of the official one using Student’s t test and F test values at 95% confidence interval level, revealing good accuracy and precision.

中文翻译：

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降解产物和剂型添加剂存在下基于丁基的反相高效液相色谱法和硅胶正相高效薄层色谱法测定帕洛诺司琼

已经开发出了稳定性指示反相高效液相色谱（RP-HPLC）和正相高效薄层色谱（NP-HPTLC）方法，用于测定帕洛诺司琼，帕洛诺司琼是一种用于化疗的强效止吐药。对帕洛诺司琼进行了强制降解研究，以研究其稳定性。使药物经受酸，碱，中性水解，氧化，热和光解条件。已经通过Advion紧凑型质谱仪进行了质量分析以阐明氧化降解物。使用缓冲液（20 mM正磷酸氢二钾，用磷酸调节至pH 2.5）：乙腈：甲醇（60:30:10，v /）在PerfectChrom 100 C4（250×4.6 mm，5μm粒径）色谱柱上进行HPLC分离v使用光电二极管阵列检测器（PAD）在210 nm下以1 mL / min的流速作为等度模式的流动相。该方法在0.1–10μg/ mL的范围内显示出足够的线性，准确性和精密度方面的灵敏度。检测限（LOD）和定量限（LOQ）分别确定为0.03μg/ mL和0.09μg/ mL。使用甲醇：氨气（10：0.5，v / v）在预先涂有60 F ₂₅₄硅胶的铝板上进行HPTLC分离）作为流动相。CAMAG扫描仪在254 nm下操作，以吸光度模式进行光密度测定。在0.1–2μg/ band的浓度范围内建立了多项式关系，LOD和LOQ分别为0.02μg/ band和0.06μg/ band。在市售小瓶中存在降解产物和添加剂的情况下，所引用的色谱方法已成功用于帕洛诺司琼的测定。按照ICH指南进行方法验证，确认要在质量控制实验室中使用的方法的鲁棒性。使用学生t检验和F法对所引用色谱方法的结果与官方方法的结果进行了统计比较。 在95％置信区间水平下的测试值，显示出良好的准确性和精确度。