Veerendra Y V S, Brahman Pradeep Kumar, Mankumare Sharad D, Ch Jayaraju, C Vinod Kumar
Department of Chemistry, Koneru Lakshmaiah Education Foundation, Vaddeswaram, Guntur, Andhra Pradesh, 522302, India.
USP-India Private Limited, Hyderabad, Telangana, 500 101, India.
Heliyon. 2024 Jul 27;10(16):e35376. doi: 10.1016/j.heliyon.2024.e35376. eCollection 2024 Aug 30.
In recent years, the field of analytical chemistry has witnessed a notable shift towards the adoption of greener chromatographic methods, aiming to minimize the environmental impact. An effective strategy involves substituting conventional harmful organic solvents with environmentally friendly alternatives, reducing the use of hazardous chemicals that contribute to environmental concerns. However, separating drug substances without the use of buffers and organic solvents presence is a big challenge. To overcome this challenge, a combination of quality-by-design (QbD) and green analytical chemistry (GAC) was employed in this study for method development. A high-performance liquid chromatography (HPLC) method was successfully developed and validated for the simultaneous determination of Nebivolol hydrochloride, Telmisartan, Valsartan, and Amlodipine besylate. The method utilized a mobile phase composed of a mixture of 0.1 % formic acid in water (pH: 2.5) and ethanol. A regular octadecyl silica (ODS) column was employed, and UV detection at 220 nm was utilized. The method exhibited linearity within the concentration range of 25-75 μg/mL for Telmisartan and 150-450 μg/mL for Nebivolol Hydrochloride, Valsartan, and Amlodipine besylate and the correlation coefficient was greater than 0.999 for all the analytes. Limits of detection (LOD) and quantification (LOQ) were determined as 0.01 and 0.04 μg/mL for Telmisartan, 0.06 and 0.20 μg/mL for Nebivolol Hydrochloride, 0.08 and 0.25 μg/mL for Amlodipine besylate, and 0.14 and 0.46 μg/mL for Valsartan, respectively. The developed method underwent thorough validation, encompassing various parameters such as linearity, accuracy, precision, LOD, LOQ, robustness, and ruggedness. The mean recovery values were observed to range between 98.86 % and 99.89 %. The accuracy demonstrated was consistently above 98.98 % for both intra-day and inter-day precisions were with the relative standard deviations less than 2 %. To establish its robustness, a quality-by-design-based experimental design (DoE) approach was implemented. Additionally, the method's environmental friendliness was evaluated using the Analytical Greenness metric (AGREE) an analytical eco scale, both confirming its alignment with sustainable practices and reduced ecological impact. The sustainability of the solvent used in the current study was evaluated by Green Solvents Selecting Tool (GSST) Further, the developed method greenness was evaluated with the green analytical tools such as Analytical method greenness score (AMGS) and using the recently released White Analytical Chemistry (WAC) using RGB assessment tool. By employing this greener approach to chromatography method, this study contributes to the ongoing efforts in analytical chemistry to promote sustainable practices and minimize the environmental footprint of analytical methods.
近年来，分析化学领域已明显转向采用更环保的色谱方法，旨在将环境影响降至最低。一种有效的策略是用环境友好型替代品取代传统的有害有机溶剂，减少使用那些引发环境问题的危险化学品。然而，在不使用缓冲剂和有机溶剂的情况下分离药物物质是一项巨大挑战。为克服这一挑战，本研究采用了质量源于设计（QbD）和绿色分析化学（GAC）相结合的方法来进行方法开发。成功开发并验证了一种高效液相色谱（HPLC）方法，用于同时测定盐酸奈必洛尔、替米沙坦、缬沙坦和苯磺酸氨氯地平。该方法使用由0.1%甲酸水溶液（pH：2.5）和乙醇组成的混合流动相。采用常规十八烷基硅胶（ODS）柱，并在220nm处进行紫外检测。该方法在替米沙坦浓度范围为25 - 75μg/mL、盐酸奈必洛尔、缬沙坦和苯磺酸氨氯地平浓度范围为150 - 450μg/mL内呈线性，所有分析物的相关系数均大于0.999。替米沙坦的检测限（LOD）和定量限（LOQ）分别测定为0.01和0.04μg/mL，盐酸奈必洛尔为0.06和0.20μg/mL，苯磺酸氨氯地平为0.08和0.25μg/mL，缬沙坦为0.14和0.46μg/mL。所开发的方法经过了全面验证，涵盖了线性、准确性、精密度、LOD、LOQ、稳健性和耐用性等各种参数。平均回收率在98.86%至99.89%之间。日内和日间精密度的准确性均始终高于98.98%，相对标准偏差小于2%。为确定其稳健性，实施了基于质量源于设计的实验设计（DoE）方法。此外，使用分析绿色度指标（AGREE）这一分析生态量表对该方法的环境友好性进行了评估，两者均证实其符合可持续实践且生态影响降低。使用绿色溶剂选择工具（GSST）对本研究中使用的溶剂的可持续性进行了评估。此外，使用分析方法绿色度评分（AMGS）等绿色分析工具以及最近发布的使用RGB评估工具的白色分析化学（WAC）对所开发方法的绿色度进行了评估。通过采用这种更环保的色谱方法，本研究为分析化学领域促进可持续实践和最小化分析方法的环境足迹的持续努力做出了贡献。
