超声辅助分散液液微萃取与超高效液相色谱串联质谱法同时测定水样中的 12 种药物。
Simultaneous determination of 12 pharmaceuticals in water samples by ultrasound-assisted dispersive liquid-liquid microextraction coupled with ultra-high performance liquid chromatography with tandem mass spectrometry.
机构信息
School of Applied Chemistry, Shenyang University of Chemical Technology, Shenyang, Liaoning, 110142, China.
School of Pharmacy, Shenyang Pharmaceutical University, Shenyang, Liaoning, 110016, China.
出版信息
Anal Bioanal Chem. 2016 Nov;408(28):8099-8109. doi: 10.1007/s00216-016-9913-1. Epub 2016 Sep 10.
A new analytical method was developed for simultaneous determination of 12 pharmaceuticals using ultrasound-assisted dispersive liquid-liquid microextraction (DLLME) followed by ultra-high performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS). Six nonsteroidal anti-inflammatory drugs (NSAIDs, ketoprofen, mefenamic acid, tolfenamic acid, naproxen, sulindac, and piroxicam) and six antibiotics (tinidazole, cefuroxime axetil, ciprofloxacin, sulfamethoxazole, sulfadiazine, and chloramphenicol) were extracted by ultrasound-assisted DLLME using dichloromethane (800 μL) and methanol/acetonitrile (1:1, v/v, 1200 μL) as the extraction and dispersive solvents, respectively. The factors affecting the extraction efficiency, such as the type and volume of extraction and dispersive solvent, vortex and ultrasonic time, sample pH, and ionic strength, were optimized. The ultrasound-assisted process was applied to accelerate the formation of the fine cloudy solution by using a small volume of dispersive solvent, which increased the extraction efficiency and reduced the equilibrium time. Under the optimal conditions, the calibration curves showed good linearity in the range of 0.04-20 ng mL (ciprofloxacin and sulfadiazine), 0.2-100 ng mL (ketoprofen, tinidazole, cefuroxime axetil, naproxen, sulfamethoxazole, and sulindac), and 1-200 ng mL (mefenamic acid, tolfenamic acid, piroxicam, and chloramphenicol). The LODs and LOQs of the method were in the range of 0.006-0.091 and 0.018-0.281 ng mL, respectively. The relative recoveries of the target analytes were in the range from 76.77 to 99.97 % with RSDs between 1.6 and 8.8 %. The developed method was successfully applied to the extraction and analysis of 12 pharmaceuticals in five kinds of water samples (drinking water, running water, river water, influent and effluent wastewater) with satisfactory results. Graphical Abstract Twelve pharmaceuticals in water samples analyted by UHPLC-MS/MS using ultrasound-assisted DLLME.
一种新的分析方法被开发出来，用于同时测定 12 种药物，使用超声辅助分散液-液微萃取（DLLME），然后进行超高效液相色谱与串联质谱（UHPLC-MS/MS）分析。6 种非甾体抗炎药（NSAIDs，酮洛芬、甲芬那酸、托芬那酸、萘普生、舒林酸和吡罗昔康）和 6 种抗生素（替硝唑、头孢呋辛酯、环丙沙星、磺胺甲噁唑、磺胺嘧啶和氯霉素）通过超声辅助 DLLME 用二氯甲烷（800 μL）和甲醇/乙腈（1:1，v/v，1200 μL）作为萃取和分散溶剂进行提取。优化了影响萃取效率的因素，如萃取和分散溶剂的类型和体积、涡旋和超声时间、样品 pH 值和离子强度等。超声辅助过程用于加速形成细小的浑浊溶液，使用小体积的分散溶剂，提高了萃取效率，缩短了平衡时间。在最佳条件下，校准曲线在 0.04-20 ng mL（环丙沙星和磺胺嘧啶）、0.2-100 ng mL（酮洛芬、替硝唑、头孢呋辛酯、萘普生、磺胺甲噁唑和舒林酸）和 1-200 ng mL（甲芬那酸、托芬那酸、吡罗昔康和氯霉素）范围内呈现良好的线性关系。该方法的检出限和定量限范围分别为 0.006-0.091 和 0.018-0.281 ng mL。目标分析物的相对回收率在 76.77-99.97%范围内，RSD 在 1.6-8.8%之间。该方法成功应用于五种水样（饮用水、自来水、河水、进水和出水废水）中 12 种药物的提取和分析，结果令人满意。
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