期刊
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
卷 408, 期 28, 页码 8099-8109出版社
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-016-9913-1
关键词
Nonsteroidal anti-inflammatory drugs; Antibiotics; Ultrasound-assisted; Dispersive liquid-liquid microextraction; Ultra-high performance liquid chromatography with tandem mass spectrometry; Water samples
资金
- National Natural Science Foundation of China [21477082, 81503029]
- Liaoning Province Educational Department [L-2014160]
- Liaoning Province Natural Science Foundation of China [2015020701]
- Large Instrument Sharing Service Construction Special of Shenyang Science and Technology Innovation Fund [F14-195-4-00]
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 mu L) and methanol/acetonitrile (1:1, v/v, 1200 mu L) 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(-1) (ciprofloxacin and sulfadiazine), 0.2-100 ng mL(-1) (ketoprofen, tinidazole, cefuroxime axetil, naproxen, sulfamethoxazole, and sulindac), and 1-200 ng mL(-1) (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(-1), 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.
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