Reem Hasan Obaydo R.H.Obaydo , Abdulsalam Ashkar , Raneem Khayyat , Salem Alhamdan , Hadeel Kallas , Mohammad Kharrat , Amir Alhaj Sakur
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引用次数: 0
摘要
建立了一种简单、准确、环保的测定佐米曲坦(ZMT)原料药及其剂型(片剂)的方法,并利用毛细管气相色谱(GC)进行了验证。用甲醇制备标准品和样品溶液,并在230 ~ 290℃的程序升温范围内优化仪器参数,总运行时间为9.0 min。苯甲硝唑(MNZB)、内标、ZMT的保留时间分别为4.89和8.11 min。色谱柱为TRB-5毛细管柱(30 m × 0.25 mm, 0.25 μm),进样量为0.5 μL,无分裂。在6.0 ~ 80.0 μg/mL范围内,校准曲线呈线性。检测限(LOD)和定量限(LOQ)分别为0.53和1.77 μg/mL,相关系数(R²)均大于0.999。该方法适用于ZMT纯品和片剂的分析,不受制剂中其它成分的干扰。方法的验证按照ICH指南进行,所有参数符合要求的验收标准。此外,采用AGREE、改进GAPI和RGB快速模型对所提出的GC方法的绿色度和可持续性进行了评价。
Development of a new green gas chromatographic method for the determination of zolmitriptan in pure and pharmaceutical preparations
A simple, accurate, and environmentally friendly method for determining raw zolmitriptan (ZMT) and its dosage form (tablets) was developed and validated using capillary gas chromatography (GC). Methanol was used to prepare the solutions of the standard and the sample, and instrument parameters were optimized with a programmed temperature ramp ranging from 230 to 290 °C, achieving a total run time of 9.0 min. The retention times for Metronidazole Benzoate (MNZB), the internal standard, and ZMT were found to be 4.89 and 8.11 min, respectively. GC separation was performed with a TRB-5 capillary column (30 m × 0.25 mm, 0.25 μm) with a 0.5 μL injection in splitless mode. The calibration curve was linear when testing a range of concentrations of 6.0–80.0 μg/mL. The limits of detection (LOD) and quantification (LOQ) were determined to be 0.53 and 1.77 μg/mL, respectively, with a correlation coefficient (R²) greater than 0.999. The method proposed was efficiently applicable to analyze pure ZMT and in tablets, showing no interference from other components of the pharmaceutical preparation. Validation of the method was done per ICH guidelines, with all parameters meeting the required acceptance criteria. Additionally, evaluation of the greenness and sustainability of the GC method proposed was performed using AGREE, modified GAPI, and the RGB fast model.