Raw data for optimization and calibration of Micellar liquid chromatography as a sustainable tool to quantify three statins in oral solid dosage forms

A method based on micellar liquid chromatography has been developed to determine rosuvastatin, lovas- tatin and simvastatin in oral solid dosage forms. Samples were solved in mobile phase up to the target concentration, filtered and directly injected. The three statins were resolved in 30 min, using an aqueous solution of 0.10 M sodium dodecyl sulfate –7.0% 1-butanol, buffered at pH 3 with 0.01 M phosphate salt as mobile phase, running under isocratic mode at 1 mL/min through a C 18 column. Detection was at 240 nm. The effect of sodium dodecyl sulfate on elution strength was more important than that of the organic solvent. The procedure was successfully validated by the guidelines of the International Coun- cil for Harmonization in terms of: specificity, linearity ( r 2 > 0.990), calibration range (1.5 - 15 mg/L for rosuvastatin, 0.5–10 mg/L for lovastatin and simvastatin), limit of detection (0.4, 0.2 and 0.15 mg/L for ro- suvastatin, lovastatin and simvastatin, respectively), trueness (98.8–101.7%), precision ( < 2.7%), carry-over effect, robustness, and stability. Values were inside the acceptance criteria of the Methods, Method Veri- fication and Validation, Food and Drug Administration-Office of Regulatory Affairs, thus ensuring the re- liability of the results. The main feature was the low proportion of organic solvent used, thus making the procedure sustainable and green. Besides, it was easy-to-conduct and with high sample-throughput, and then useful for routine analysis in pharmaceutical quality control. Finally, it was applied to commercial pharmaceutical preparations.本研究建立了一种基于胶束液相色谱法（micellar liquid chromatography）的分析方法，用于测定口服固体制剂中的瑞舒伐他汀、洛伐他汀与辛伐他汀。将样品用流动相溶解至目标浓度后过滤，直接进样分析。三种他汀类药物可在30分钟内实现分离，所用流动相为含0.10 M十二烷基硫酸钠（sodium dodecyl sulfate）与7.0%正丁醇（1-butanol）的水溶液，以0.01 M磷酸盐缓冲液调节至pH 3，采用等度洗脱模式，流速为1 mL/min，色谱柱为C18柱（C18 column），检测波长设定为240 nm。十二烷基硫酸钠对洗脱强度的影响显著大于有机溶剂。本方法依据国际人用药品注册技术协调会（International Council for Harmonization, ICH）指南完成验证，验证指标包括专属性、线性（决定系数r²>0.990）、校准范围（瑞舒伐他汀为1.5~15 mg/L，洛伐他汀与辛伐他汀为0.5~10 mg/L）、检出限（瑞舒伐他汀、洛伐他汀、辛伐他汀分别为0.4、0.2、0.15 mg/L）、正确度（98.8%~101.7%）、精密度（<2.7%）、残留效应、耐用性与稳定性。所有验证结果均符合美国食品药品监督管理局（Food and Drug Administration, FDA）监管事务办公室发布的《方法验证与确认》指南的接受标准，确保了实验结果的可靠性。本方法的核心优势在于有机溶剂用量极低，具备可持续性与绿色分析特性；此外，该方法操作简便、样品通量高，可用于药品质量控制中的常规分析工作。最后，本方法已应用于市售药物制剂的实际检测。