College of Science, Beijing University of Chemical Technology, Beijing 100029, China.
Talanta. 2013 May 15;109:177-84. doi: 10.1016/j.talanta.2013.02.048. Epub 2013 Mar 4.
In this study, a two-phase hollow fiber liquid-phase microextraction (HF-LPME) coupling with ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed for determination of four non-steroidal anti-inflammatory (NSAIDs)-salicylic acid, ibuprofen, naproxen and diclofenac in real water samples. The influencing parameters of HF-LPME sample preparation method, such as organic solvents (acceptor phase), pH of sample solution (donor phase), extraction time, stirring speed, extraction temperature and ionic strength were systematically optimized. Through the developed determination method, high enrichment factors (195-346) were achieved for the four drugs. The instrumental calibration curves of salicylic acid, naproxen, diclofenac, and ibuprofen show good linear relations (R>0.998) in the concentration range of 1-500, 5-2500, 10-5000 and 5-2500 μg L(-1), respectively. The average recoveries of the four drugs in the low, medium and high spiked concentration levels (20-200, 50-500 and 100-1000 μg L(-1)) were between 98-115% with relative standard deviation (RSD) values were less than 12% (n=6). Limits of detection (LOD) of salicylic acid, naproxen, diclofenac, and ibuprofen in water were 0.5, 0.5, 1.0, and 1.25 μg L(-1), respectively. The determination method has been applied for the real samples (purified water, tap water, juice, soda and energy drinks), and the results show that salicylic acid was detected in tap water and soda, the concentrations were 2.85 μg L(-1) and 61.22 μg L(-1) separately, the RSD values were less than 9% (n=6). Salicylic acid and diclofenac were detected in energy drink, the concentrations were 44.62 μg L(-1) and 8.31 μg L(-1), the RSD values were less than 11% (n=6).
在这项研究中,开发了一种两相中空纤维液相微萃取(HF-LPME)与超高效液相色谱串联质谱(UPLC-MS/MS)联用的方法,用于测定真实水样中的四种非甾体抗炎药(NSAIDs)-水杨酸、布洛芬、萘普生和双氯芬酸。系统优化了 HF-LPME 样品制备方法的影响参数,如有机溶剂(受体相)、样品溶液的 pH 值(供体相)、萃取时间、搅拌速度、萃取温度和离子强度。通过开发的测定方法,四种药物均获得了高的富集因子(195-346)。水杨酸、萘普生、双氯芬酸和布洛芬的仪器校准曲线在 1-500、5-2500、10-5000 和 5-2500μg L(-1) 的浓度范围内均表现出良好的线性关系(R>0.998)。四种药物在低、中、高浓度水平(20-200、50-500 和 100-1000μg L(-1))的平均回收率在 98-115%之间,相对标准偏差(RSD)值小于 12%(n=6)。水杨酸、萘普生、双氯芬酸和布洛芬在水中的检出限(LOD)分别为 0.5、0.5、1.0 和 1.25μg L(-1)。该测定方法已应用于实际样品(纯净水、自来水、果汁、苏打水和能量饮料),结果表明,自来水中检出水杨酸,浓度为 2.85μg L(-1),苏打水中检出水杨酸,浓度为 61.22μg L(-1),RSD 值小于 9%(n=6)。能量饮料中检出水杨酸和双氯芬酸,浓度分别为 44.62μg L(-1)和 8.31μg L(-1),RSD 值小于 11%(n=6)。