Department of Pharmaceutical Analysis, GITAM Institute of Pharmacy, Gandhi Institute of Technology and Management (GITAM) (Deemed to be University), Visakhapatnam, Pin code: 530 045, Andhra Pradesh (State), India.
Arch Razi Inst. 2024 Feb 1;79(1):68-82. doi: 10.32592/ARI.2024.79.1.68. eCollection 2024 Feb.
Selenium is a class 2B element according to the International Council for Harmonization Q3D guidelines. Selenium sulfide is an anti-infective agent with antifungal and antibacterial properties used to treat dandruff and seborrheic dermatitis. The literature survey revealed that most of the analytical techniques to estimate selenium were time-consuming and/or required high skill levels. The process involved identifying the isotopes, selecting the measurement approach, and optimizing a typical microwave-aided digesting procedure. Ammonium hydrogen difluoride, water, and concentrated nitric acid were added to the samples. The confirmed microwave digestion program was a two-step program where in the initial step, the samples were ramped at 200°C for 20 min and held for 5 min. Later, samples were cooled and neutralized by boric acid, then ramped for 20 min to a temperature of 180°C and held for 10 min. Selenium was estimated at 196.090 nm by inductively coupled plasma optical emission spectroscopy (ICP-OES). System suitability was run before initiating analysis to ensure that system performance was consistent. Analytical validation parameters, such as the specificity of the method, were demonstrated at 196.090 nm, linearity was proven from 10 ppm to 150 ppm of selenium concentration, the detection limit was 1.28 ppm, and the limit of quantification was 3.89 ppm. Robustness was confirmed for small changes to ICP-OES operating conditions. The precision of the method demonstrated by analyzing the percentage relative standard deviation for six injections was found to be less than 2.0%. Accuracy was confirmed from 10 ppm to 150 ppm, and all the samples were observed to be within the range of 95%-105%. A common microwave-assisted digestion technique was developed and validated as well. The precision, specificity, linearity, accuracy, and robustness of the method for estimating selenium in selenium sulfide drug substances and various pharmaceutical dosage forms were demonstrated. This newly developed microwave-assisted digestion technique has optimum sensitivity and is highly reproducible and time-saving than the existing methods This method can be applied to numerous matrices for a finished dosage of selenium sulfide formulations.
根据国际协调理事会 Q3D 指南，硒是 2B 类元素。二硫化硒是一种具有抗真菌和抗菌特性的抗感染药物，用于治疗头皮屑和脂溢性皮炎。文献调查显示，大多数用于估计硒的分析技术都很耗时，并且/或者需要高水平的技能。该过程涉及识别同位素、选择测量方法以及优化典型的微波辅助消解程序。将样品中加入了氟化氢铵、水和浓硝酸。经确认的微波消解程序为两步程序，其中在初始步骤中，将样品以 200°C 升温 20 分钟，保持 5 分钟。然后，冷却样品并用硼酸中和，然后以 180°C 升温 20 分钟并保持 10 分钟。通过电感耦合等离子体光学发射光谱法（ICP-OES）在 196.090nm 处估计硒。在开始分析之前进行系统适用性测试，以确保系统性能一致。在 196.090nm 处证明了方法的特异性等分析验证参数，从 10ppm 到 150ppm 的硒浓度证明了线性关系，检测限为 1.28ppm，定量限为 3.89ppm。确认了对 ICP-OES 操作条件的微小变化的稳健性。通过分析六个进样的百分比相对标准偏差来证明该方法的精密度，发现小于 2.0%。从 10ppm 到 150ppm 确认了准确性，所有样品均在 95%-105%范围内。还开发并验证了一种常见的微波辅助消解技术。该方法在测定二硫化硒药物制剂和各种药物剂型中的硒含量方面表现出了良好的精密度、特异性、线性、准确性和稳健性。这种新开发的微波辅助消解技术具有最佳的灵敏度，比现有方法更具重现性和节省时间。该方法可应用于众多的硒硫化物制剂的基质中。
