Green homogeneous liquid-liquid microextraction (HLLME) under high salinity conditions was proposed for the determination of nimesulide in human urine. The proposed analytical scheme consisted of the mixing of the appropriate volume of acetonitrile and sample followed by the addition of Na₂SO₄ solution to obtain phase separation. Following the extraction of the drug from the urine samples, high-performance chromatography-diode array detection (HPLC-PDA) was used for its determination. The main factors influencing the performance of the HLLME method were studied and optimized using a two-step experimental design (Plackett-Burman, Central Composite Design). The HLLME-HPLC-PDA method was systematically validated using the accuracy profiles. The detection limit was adequate and estimated to be 0.03 μg mL⁻¹. The mean analytical bias (expressed as relative error) ranged between ─ 2.9–3.6% and the relative standard deviation (RSD) was better than 3.7%. Moreover, the β-expectation tolerance intervals were in the range of ±15% demonstrating that 95% of the results will fall within the defined bias limits. The ruggedness of the herein developed protocol was assessed using Monte-Carlo simulations followed by capability analysis. The proposed scheme was applied for the determination of the drug in real urine samples following the administration of pharmaceutical formulations that contained nimesulide.

提出了高盐度条件下的绿色均相液-液微萃取 (HLLME) 测定人尿中尼美舒利的方法。建议的分析方案包括混合适当体积的乙腈和样品，然后加入 Na ₂ SO ₄溶液获得相分离。从尿液样品中提取药物后，使用高效色谱-二极管阵列检测 (HPLC-PDA) 对其进行测定。使用两步实验设计（Plackett-Burman，Central Composite Design）研究和优化了影响 HLLME 方法性能的主要因素。使用准确度曲线系统地验证了 HLLME-HPLC-PDA 方法。检测限足够，估计为0.03 μg mL ^-1。平均分析偏差（表示为相对误差）介于 ─ 2.9-3.6% 之间，相对标准偏差 (RSD) 优于 3.7%。此外，β- 预期容差区间在 ±15% 的范围内，表明 95% 的结果将落在定义的偏差范围内。本文开发的协议的耐用性使用蒙特卡罗模拟进行评估，然后进行能力分析。所提出的方案用于在施用含有尼美舒利的药物制剂后测定真实尿液样品中的药物。