Batool Hafiza Monaza, Jalees Muhammad Irfan, Batool Madeeha
School of Chemistry, University of the Punjab, Lahore 54590, Pakistan.
Institute of Environmental Engineering and Research, University of Engineering and Technology, Lahore 54890, Pakistan.
Toxicol Rep. 2024 Oct 9;13:101763. doi: 10.1016/j.toxrep.2024.101763. eCollection 2024 Dec.
Glucocorticoids are widely used as highly effective drugs for treating inflammatory diseases. In this study, a method was developed and validated using liquid chromatography-tandem mass spectrometry (LC-MS/MS) to simultaneously determine four glucocorticoids, including betamethasone, dexamethasone, hydrocortisone, and prednisolone in unauthorized or unregulated medicinal powders often associated with quackery formulations. Commercially available standards were used for method development and glucocorticoid detection. Glucocorticoids were extracted from the samples with methanol, which were then chromatographically separated using two mobile phases (0.1 % formic acid in water and 0.1 % formic acid in acetonitrile) in an isocratic flow on an Agilent Poroshel 120 C18 column (2.1 mm x 75 mm x 2.7 m). The validated analytical measuring range (AMR) of betamethasone and dexamethasone was 7.8-500 ng/mL, whereas, for hydrocortisone and prednisolone, AMR was 7.8-1000 ng/mL. The method showed an excellent coefficient of determination (r2) >0.990 for betamethasone, hydrocortisone, and prednisolone, while for dexamethasone 0.986. Accuracy and precision (intra/inter days) of these glucocorticoids showed a bias of 6-15 % (<20 %) and a coefficient of variation (CV) of <15 %. For each dilution factor, the integrity of samples was maintained after dilution. The developed method is sensitive and valuable for detecting, quantifying, and confirming the selected glucocorticoids in various quackery formulation powders commonly used in Pakistani setups.
糖皮质激素作为治疗炎症性疾病的高效药物被广泛使用。在本研究中，开发并验证了一种使用液相色谱 - 串联质谱法（LC-MS/MS）同时测定四种糖皮质激素的方法，这四种糖皮质激素包括倍他米松、地塞米松、氢化可的松和泼尼松龙，它们存在于常与江湖郎中配方相关的未经授权或不受监管的药粉中。使用市售标准品进行方法开发和糖皮质激素检测。用甲醇从样品中提取糖皮质激素，然后在安捷伦Poroshel 120 C18柱（2.1 mm×75 mm×2.7 µm）上采用等度洗脱，使用两种流动相（水中0.1%甲酸和乙腈中0.1%甲酸）进行色谱分离。倍他米松和地塞米松的验证分析测量范围（AMR）为7.8 - 500 ng/mL，而氢化可的松和泼尼松龙的AMR为7.8 - 1000 ng/mL。该方法对于倍他米松、氢化可的松和泼尼松龙显示出优异的测定系数（r2）>0.990，而地塞米松为0.986。这些糖皮质激素的准确度和精密度（日内/日间）偏差为6 - 15%（<20%），变异系数（CV）<15%。对于每个稀释因子，稀释后样品的完整性得以保持。所开发的方法对于检测、定量和确证巴基斯坦常见的各种江湖郎中配方药粉中选定的糖皮质激素具有敏感性和价值。
