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.本研究开发了一种基于胶束液相色谱（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并定容至目标浓度，经过滤后直接进样。以0.10 M十二烷基硫酸钠（sodium dodecyl sulfate）-7.0%正丁醇（1-butanol）水溶液（以0.01 M磷酸盐缓冲盐调节至pH 3.0）作为流动相，采用等度洗脱模式，流速1 mL/min，流经C18色谱柱，可在30分钟内实现三种他汀类药物的基线分离。检测波长设定为240 nm。研究发现，十二烷基硫酸钠对洗脱强度的影响显著大于有机溶剂。本方法依据人用药品注册技术要求国际协调会（International Council for Harmonization, ICH）指南完成系统验证，验证指标涵盖专属性、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均为0.5~10 mg/L）、检出限（瑞舒伐他汀、洛伐他汀、辛伐他汀依次为0.4、0.2、0.15 mg/L）、准确度（98.8%~101.7%）、精密度（<2.7%）、残留效应、耐用性与稳定性。所有验证参数均符合美国食品药品监督管理局监管事务办公室（Food and Drug Administration-Office of Regulatory Affairs, FDA-ORA）发布的《方法验证与确认》指南的接收标准，确保了实验结果的可靠性。该方法的核心优势在于有机溶剂使用占比极低，具备可持续性与绿色环保特性。此外，本方法操作简便、样品通量高，可有效应用于药品质量控制中的常规分析工作。最后，本方法已成功应用于市售药物制剂的检测分析。