Shah C R, Suhagia B N, Shah N J, Patel D R, Patel N M
Department of Quality Assurance, Shri B. M. Shah College of Pharmaceutical Education and Research, College Campus, Modasa-383 315, India.
Indian J Pharm Sci. 2008 Mar-Apr;70(2):251-5. doi: 10.4103/0250-474X.41469.
A rapid, selective and stability-indicating high performance thin layer chromatographic method was developed and validated for the simultaneous estimation of olanzapine and fluoxetine in combined tablet dosage form. Olanzapine and fluoxetine were chromatographed on silica gel 60 F(254) TLC plate using methanol:toluene (4:2 v/v) as the mobile phase and spectrodensitometric scanning-integration was performed at a wavelength of 233 nm using a Camag TLC Scanner III. This system was found to give compact spots for both olanzapine (R(f) value of 0.63+/-0.01) and fluoxetine (R(f) value of 0.31+/-0.01). The polynomial regression data for the calibration plots showed good linear relationship with r(2)=0.9995 in the concentration range of 100-800 ng/spot for olanzapine and 1000-8000 ng/spot for fluoxetine with r(2)=0.9991. The method was validated in terms of linearity, accuracy, precision, recovery and specificity. The limit of detection and the limit of quantification for the olanzapine were found to be 30 and 100 ng/spot, respectively and for fluoxetine 300 and 1000 ng/spot, respectively. Olanzapine and fluoxetine were degraded under acidic, basic and oxidation degradation conditions which showed all the peaks of degraded product were well resolved from the active pharmaceutical ingredient. Both drugs were not further degraded after thermal and photochemical degradation. The method was found to be reproducible and selective for the simultaneous estimation of olanzapine and fluoxetine. As the method could effectively separate the drugs from their degradation products, it can be employed as a stability-indicating method.
建立并验证了一种快速、选择性且具有稳定性指示功能的高效薄层色谱法，用于同时测定复方片剂剂型中奥氮平和氟西汀的含量。奥氮平和氟西汀在硅胶60 F(254) TLC板上进行色谱分离，以甲醇:甲苯(4:2 v/v)为流动相，使用Camag TLC Scanner III在233 nm波长下进行光密度扫描积分。该系统对奥氮平（R(f)值为0.63±0.01）和氟西汀（R(f)值为0.31±0.01）均给出了清晰的斑点。校准曲线的多项式回归数据显示，奥氮平在100 - 800 ng/斑点浓度范围内，r(2)=0.9995，氟西汀在1000 - 8000 ng/斑点浓度范围内，r(2)=0.9991，均呈现良好的线性关系。该方法在线性、准确度、精密度、回收率和专属性方面得到了验证。奥氮平的检测限和定量限分别为30和100 ng/斑点，氟西汀的检测限和定量限分别为300和1000 ng/斑点。奥氮平和氟西汀在酸性、碱性和氧化降解条件下均发生降解，结果表明所有降解产物的峰均与活性药物成分良好分离。热降解和光化学降解后，两种药物均未进一步降解。该方法被发现对于同时测定奥氮平和氟西汀具有可重复性和选择性。由于该方法能够有效地将药物与其降解产物分离，因此可作为一种稳定性指示方法。
