Sava Healthcare Limited, (Research and Development Center), Chinchwad MIDC, Pune, 411019, India.
J AOAC Int. 2023 Jul 17;106(4):866-872. doi: 10.1093/jaoacint/qsad036.
Azelastine HCl (AZ) and fluticasone propionate (FL) nasal spray drug product is commonly used in the treatment of allergic rhinitis worldwide. To date, the impurity profiling of this product has not been reported.
The present study aimed to develop and validate a novel RP-HPLC stability-indicating analytical method for the estimation of impurities from AZ and FL nasal spray drug product.
A mixture of octane sulfonic acid sodium salt and trifluroacetic acid is used as a mobile phase A. Acetonitrile is used as a mobile phase B. Good separation was achieved on Baker bond phenyl hexyl, 250 × 4.6, 5 µm column at 1 mL/min flow rate in gradient elution mode. The chromatograms were monitored at 239 nm.
The LOD and LOQ were found to be 0.006 and 0.019 µg/mL for AZ and 0.010 and 0.030 µg/mL for FL, respectively. The correlation coefficient for all the known impurities and principal analytes was 0.999 from LOQ level to 150% of standard concentration. The recovery for all the known impurities was found to be between 90 and 110%. In the stress study, 15% degradation was observed in basic conditions and 8.7% in acidic conditions. No significant degradation was observed in thermal and oxidative conditions.
An impurity profiling method for AZ and FL combination nasal spray product was successfully developed, validated, and demonstrated to be accurate, precise, specific, robust, and stability-indicating. The method can be routinely used for impurity testing of commercial batches in QC laboratories in the pharmaceutical industry.
No impurity study has been reported for this combination product until now.
盐酸氮卓斯汀（AZ）和丙酸氟替卡松（FL）鼻喷雾剂药物在全球范围内常用于治疗过敏性鼻炎。迄今为止，尚未报道该产品的杂质分析情况。
本研究旨在开发和验证一种新的反相高效液相色谱法（RP-HPLC），用于测定 AZ 和 FL 鼻喷雾剂药物的杂质。
混合使用辛烷磺酸钠盐和三氟乙酸作为流动相 A，乙腈作为流动相 B。在梯度洗脱模式下，以贝克邦尔苯基己基，250×4.6，5μm 柱为固定相，以 1mL/min 的流速进行分离。在 239nm 处监测色谱图。
AZ 的检测限（LOD）和定量限（LOQ）分别为 0.006 和 0.019μg/mL，FL 的分别为 0.010 和 0.030μg/mL。所有已知杂质和主成分的相关系数均在 0.999 以上，LOQ 至 150%标准浓度范围内。所有已知杂质的回收率在 90%至 110%之间。在稳定性研究中，碱性条件下观察到 15%的降解，酸性条件下观察到 8.7%的降解。在热和氧化条件下未观察到明显降解。
成功开发、验证了一种用于 AZ 和 FL 联合鼻喷雾剂产品的杂质分析方法，该方法准确、精密、专属性强、耐用且具有稳定性指示作用。该方法可在制药行业的 QC 实验室中常规用于商业批次的杂质检测。
到目前为止，尚未有关于该联合产品的杂质研究报道。
