背景:托芬那酸(TA)属于非甾体类抗炎药。关于用于TA测定的可靠且经过验证的稳定性指示方法的可用性的信息不足。
目标:一个相对简单的,快速,准确,精确,经济,健壮,已开发出指示稳定性的RP-HPLC方法来测定纯剂型和片剂剂型中的TA。
方法:该方法根据ICH指南进行了验证,和线性等参数,范围,选择性,准确度,精度,鲁棒性,特异性,并测定了溶液的稳定性。使用TLC和FTIR光谱法确定TA的纯度。用已知的杂质和进行强制降解后,而稳健性是由Plackett-Burman的实验设计建立的。用于分析的流动相为乙腈和pH为2.5的水(90:10,v/v)。使用C18柱在280nm处进行活性药物的检测(tR=4.3min。).还检查了TA的黄色多晶型形式的方法的适用性。
结果:结果表明,该方法具有很高的准确性(99.39-100.80%),精确(<1.5%RSD),稳健(<2%RSD),并与英国药典方法具有统计学可比性,具有更好的敏感性和特异性。
结论:观察到应力降解研究不影响该方法的准确性和特异性。因此,所提出的方法可用于测定TA及其片剂剂型。
BACKGROUND: Tolfenamic acid (TA) belongs to the fenamates class of nonsteroidal anti-inflammatory drugs. Insufficient information is available regarding the availability of a reliable and validated stability-indicating method for the assay of TA.
OBJECTIVE: A relatively simple, rapid, accurate, precise, economical, robust, and stabilityindicating RP-HPLC method has been developed to determine TA in pure and tablet dosage forms.
METHODS: The method was validated according to the ICH guideline, and parameters like linearity, range, selectivity, accuracy, precision, robustness, specificity, and solution stability were determined. TLC and FTIR spectrometry were used to ascertain the purity of TA. The specificity was determined with known impurities and after performing forced degradation, while the robustness was established by Plackett-Burman\'s experimental design. The mobile phase used for the analysis was acetonitrile and water (90:10, v/v) at pH 2.5. The detection of the active drug was made at 280 nm using a C18 column (tR = 4.3 min.). The method\'s applicability was also checked for the yellow polymorphic form of TA.
RESULTS: The results indicated that the method is highly accurate (99.39-100.80%), precise (<1.5% RSD), robust (<2% RSD), and statistically comparable to the British Pharmacopoeia method with better sensitivity and specificity.
CONCLUSIONS: It was observed that the stress degradation studies do not affect the method\'s accuracy and specificity. Hence the proposed method can be used to assay TA and its tablet dosage form.