Barfi Behruz, Asghari Alireza, Rajabi Maryam, Goochani Moghadam Ahmad, Mirkhani Nasim, Ahmadi Farhad
Department of Chemistry, Semnan University, Semnan 35195-363, Iran.
Department of Chemistry, Semnan University, Semnan 35195-363, Iran.
J Pharm Biomed Anal. 2015;111:297-305. doi: 10.1016/j.jpba.2015.03.034. Epub 2015 Apr 13.
Two dispersive-based liquid-liquid microextraction methods including ultrasound-enhanced air-assisted liquid-liquid microextraction (USE-AALLME) and low-density solvent-based dispersive liquid-liquid microextraction (LDS-DLLME) were compared for the extraction of salicylic acid (the hydrolysis product of acetylsalicylic acid), diclofenac and ibuprofen, as instances of the most commonly used nonsteroidal anti-inflammatory drugs (NSAIDs), in human urine prior to their determination by gas chromatography with flame ionization detection (GC-FID). The influence of different parameters affecting the USE-AALLME (including type and volume of the extraction solvent, sample pH, ionic strength, and simultaneous sonication and number of extraction cycles) and the LDS-DLLME (including type and volume of the extraction and disperser solvents, sample pH, and ionic strength) were investigated to optimize their extraction efficiencies. Both methods are fast, simple and convenient with organic solvent consumption at μL level. However, the best results were obtained using the USE-AALLME method, applying 30 μL of 1-octanol as extraction solvent, 5.0 mL of sample at pH 3.0, without salt addition, and 5 extraction cycles during 20s of sonication. This method was validated based on linearities (r(2) >0 .971), limits of detection (0.1-1.0 μg L(-1)), linear dynamic ranges (0.4-1000.0 μg L(-1)), enrichment factors (115 ± 3-135 ± 3), consumptive indices (0.043-0.037), inter- and intra-day precisions (4.3-4.8 and 5.6-6.1, respectively), and relative recoveries (94-103%). The USE-AALLME in combination with GC-FID, and with no need to derivatization step, was demonstrated to be a simple, inexpensive, sensitive and efficient method to determine NSAIDs in human urine samples.
比较了两种基于分散液液微萃取的方法，即超声强化空气辅助液液微萃取（USE-AALLME）和低密度溶剂基分散液液微萃取（LDS-DLLME），用于在通过火焰离子化检测气相色谱法（GC-FID）测定之前，从人尿中萃取水杨酸（乙酰水杨酸的水解产物）、双氯芬酸和布洛芬，这些是最常用的非甾体抗炎药（NSAIDs）的实例。研究了影响USE-AALLME（包括萃取溶剂的类型和体积、样品pH值、离子强度以及同时进行的超声处理和萃取循环次数）和LDS-DLLME（包括萃取和分散溶剂的类型和体积、样品pH值和离子强度）的不同参数的影响，以优化它们的萃取效率。两种方法都快速、简单且方便，有机溶剂消耗为微升水平。然而，使用USE-AALLME方法获得了最佳结果，采用30 μL 1-辛醇作为萃取溶剂，5.0 mL pH为3.0的样品，不添加盐，并在20 s超声处理期间进行5次萃取循环。该方法基于线性关系（r(2) >0.971）、检测限（0.1 - 1.0 μg L(-1)）、线性动态范围（0.4 - 1000.0 μg L(-1)）、富集因子（115 ± 3 - 135 ± 3）、消耗指数（0.043 - 0.037）、日内和日间精密度（分别为4.3 - 4.8和5.6 - 6.1）以及相对回收率（94 - 103%）进行了验证。USE-AALLME与GC-FID联用，无需衍生化步骤，被证明是一种简单、廉价、灵敏且高效的测定人尿样中NSAIDs的方法。
