Rao Janhavi, Chauhan Kanchan, Mahadik K R, Kadam S S
Department of Pharmaceutical Chemistry, Poona College of Pharmacy, Bharati Vidyapeeth University, Erandwane, Pune - 411 038, India.
Indian J Pharm Sci. 2009 Jan;71(1):24-9. doi: 10.4103/0250-474X.51946.
A stability-indicating HPLC method was developed and validated for the quantitative determination of diacerein in capsule dosage forms. An isocratic separation was achieved using a perfectsil target ODS-3, 250x4.6 mm i.d., 5 microm particle size columns with a flow rate of 1 ml/min and using a UV detector to monitor the eluate at 254 nm. The mobile phase consisted of phosphate buffer:acetonitrile (40:60, v/v) with pH 4.0 adjusted with phosphoric acid. The drug was subjected to oxidation, hydrolysis, photolysis and thermal degradation. Diacerein was found to degrade in acidic, basic, and oxidative stress and also under neutral condition. Complete separation of degraded products was achieved from the parent compound. All degradation products in an overall analytical run time of approximately 10 min with the parent compound diacerein eluting at approximately 4.9 min. The method was linear over the concentration range of 1-10 microg/ml (r(2) = 0.9996) with a limit of detection and quantitation of 0.01 and 0.05 microg/ml respectively. The method has the requisite accuracy, selectivity, sensitivity, precision and robustness to assay diacerein in capsules. Degradation products resulting from the stress studies did not interfere with the detection of diacerein and the assay is thus stability-indicating.
建立了一种用于定量测定胶囊剂型中双醋瑞因的稳定性指示高效液相色谱法并进行了验证。使用粒径为5微米、内径250×4.6毫米的Perfectsil Target ODS-3色谱柱，以1毫升/分钟的流速进行等度分离，并用紫外检测器在254纳米处监测洗脱液。流动相由磷酸盐缓冲液：乙腈（40:60，v/v）组成，用磷酸调节pH值至4.0。对该药物进行了氧化、水解、光解和热降解实验。发现双醋瑞因在酸性、碱性和氧化应激条件下以及中性条件下均会降解。降解产物与母体化合物实现了完全分离。在大约10分钟的总分析运行时间内，所有降解产物均被分离，母体化合物双醋瑞因在约4.9分钟时洗脱。该方法在1-10微克/毫升的浓度范围内呈线性（r(2)=0.9996），检测限和定量限分别为0.01和0.05微克/毫升。该方法具有测定胶囊中双醋瑞因所需的准确度、选择性、灵敏度、精密度和稳健性。应激研究产生的降解产物不干扰双醋瑞因的检测，因此该测定方法具有稳定性指示作用。
