两种快速灵敏方法测定片中替诺昔康含量的比较研究

Ashutosh Kumar Singh, P. García, F. Gomes, É. Kedor-Hackmann, M. Santoro
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引用次数: 4

摘要

替诺昔康是吡罗西康的类似物,是一种非甾体抗炎药。它用于骨关节炎和类风湿性关节炎等肌肉骨骼和关节疾病的症状管理,也用于软组织损伤的短期管理。其在制剂中的定量测定对于保证理想的治疗效果具有重要意义。本研究的目的是建立、验证和比较分光光度法和色谱法定量测定片剂中替诺昔康的方法。在这项工作中,分析了不同来源的含有20.0 mg替诺昔康的片剂。以0.1 mol/L NaOH为溶剂,在368 nm处取信号,验证了分光光度法的有效性。采用Synergi Hydro-RP®C18色谱柱(250x4.6 mm, 4µm)对HPLC法进行验证。流动相为甲醇-水(61:39 v/v),用甲酸调节pH为2.5,流速为1.0 mL/min。在375 nm处进行紫外检测。所有分析均在柱温为25°C±1的条件下进行。在4.0 ~ 24.0µg/mL范围内,校准曲线呈线性关系,相关系数大于0.9999。紫外法的检出限(DL)和定量限(QL)分别为0.25µg/mL和0.90µg/mL,高效液相色谱法的检出限(QL)分别为0.35µg/mL和1.20µg/mL。两种方法的日内和日内精度均低于2%,以RSD表示。紫外法和高效液相色谱法对替诺昔康的平均回收率分别为98.5 ~ 101.25%和99.01 ~ 101.93%。紫外法和高效液相色谱法快速、准确、精密度高。紫外分光光度法与高效液相色谱法在统计学上无显著差异。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Comparative study on two rapid and sensitive methods for quantitative determination of tenoxicam in tablets
Tenoxicam, a piroxicam analogue, is an NSAID (Non-Steroid Antinflamatory Drug). It is used in the symptomatic management of musculoskeletal and joint disorders such as osteoarthritis and rheumatoid arthritis, and also in the short-term management of soft-tissue injury. Its quantitative determination in pharmaceutical formulations is important to guarantee the desired therapeutic effects. The objective of this research was to develop, validate and compare spectrophotometric and chromatographic methods in the quantitative determination of tenoxicam in tablet preparations. In this work, tablets containing 20.0 mg of tenoxicam from different origins were analyzed. The spectrophotometric method was validated using 0.1 mol/L NaOH as solvent and a signal at 368 nm was taken. The HPLC method was validated using Synergi Hydro-RP® C18 column (250x4.6 mm, 4 µm). The mobile phase was constituted of methanol-water (61:39 v/v) with pH adjusted to 2.5 with formic acid, at a flow rate of 1.0 mL/min. UV detection was made at 375 nm. All analyses were performed with a column temperature of 25 °C ± 1. The calibration curves were linear over a concentration range from 4.0-24.0 µg/mL with a correlation coefficient better than 0.9999. The detection limit (DL) and quantitation limit (QL) were 0.25 µg/mL and 0.90 µg/mL for UV method and 0.35 µg/mL and 1.20 µg/mL for HPLC method respectively. The intra-day and inter-day precision expressed as RSD were below 2% for both methods. The mean recovery of tenoxicam was found to be in the range of 98.5-101.25% for UV method and 99.01-101.93% for HPLC method. The UV and HPLC methods were found to be rapid, precise and accurate. Statistically there was no significant difference between proposed UV spectrophotometric and HPLC methods.
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