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《Biomedical chromatography : BMC》2018,32(6)
A molecularly imprinted polymer was synthesized and applied as a sorbent in the solid‐phase extraction device. The imprinted polymer was characterized by fourier‐transform infrared spectroscopy and scanning electron microscope. The results revealed that imprinted polymer possess sensitive selectivity and reliable adsorption properties for five NSAIDs. The imprinted polymer was successfully applied to the pre‐concentration for five NSAIDs in different water samples prior to UPLC‐MS/MS. In the early studies, several factors were investigated, including pH adjustment, the kind of elution solvent and the volume of elution solvent. Finally, we found that the pH 5 and an aliquot of 2 mL methanol were suitable for the water samples. The limits of detection and limits of quantitation of five nonsteroidal anti‐inflammatory drugs varied from 0.007 to 0.480 μg L−1 and 0.03 to 1.58 μg L−1, respectively. The spiking recoveries of the target analytes were 50.33‐127.64% at the levels of 0.2 μg L−1, 2 μg L−1 and 5 μg L−1. The precision and accuracy of this method showed a great increase compared with traditional solid‐phase extraction. The developed method was successfully applied to extraction and analysis of NSAIDs in different water samples with satisfactory results which could help us better understand their environmental fate and risk to ecological health. 相似文献
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Moustafa A. Gouda 《合成通讯》2017,47(17):1527-1558
The biological and medicinal properties of oxicams and its analogues have prompted enormous research aimed at developing synthetic routes to these heterocycles. This review focuses on the chemical properties associated with this system. 相似文献
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Determination of four acidic nonsteroidal anti‐inflammatory drugs in wastewater samples by dispersive liquid–liquid microextraction based on solidification of floating organic droplet and high‐performance liquid chromatography 下载免费PDF全文
Mihail Simion Beldean‐Galea Virginia Coman Didier Thiébaut Jérome Vial 《Journal of separation science》2015,38(4):641-648
A simple, environmentally friendly, and sensitive dispersive liquid–liquid microextraction based on solidification of floating organic droplet for the extraction of four acidic nonsteroidal anti‐inflammatory drugs (ketoprofen, naproxen, ibuprofen, and diclofenac) from wastewater samples subsequent by high‐performance liquid chromatography analysis was developed. The influence of extraction parameters such as pH, the effect of solution ionic strength, type of extraction solvent, disperser solvent, and extraction solvent volume were studied. High enrichment factors (283–302) were obtained through the developed method. The method provides good linearity (r > 0.999) in a concentration range of 1–100 μg/L, good intra‐ and inter‐day precision (relative standard deviation < 7%) and low limits of quantification. The relative recoveries of the selected compounds were situated over 80% both in synthetic and real water samples. The developed method has been successfully applied for the analysis of the selected compounds in wastewater samples. 相似文献
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本文建立了一种快速的微薄辅助萃取-高效液相色谱法分离检测羊肝、牛肉和牛奶样品中三种喹诺酮类药物(氟罗沙星、洛美沙星和斯帕沙星)和两种非甾类化合物(酮洛芬和布洛芬)的方法。并对微波辅助萃取条件利用正交试验进行了优化:萃取温度为4℃、萃取时间为6min、萃取溶剂为乙腈、萃取溶剂体积为10mL。在浓度范围为0.25—0.75 μg•g-1时各待测物的三种不同水平的添加回收率在60.0%到107%之间,并获得较好的精确度(RSD<11%)。 相似文献
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Janine N. Boodram Iain J. Mcgregor Peter M. Bruno Paul B. Cressey Dr. Michael T. Hemann Dr. Kogularamanan Suntharalingam 《Angewandte Chemie (International ed. in English)》2016,55(8):2845-2850
The breast cancer stem cell (CSC) potency of a series of copper(II)–phenanthroline complexes containing the nonsteroidal anti‐inflammatory drug (NSAID), indomethacin, is reported. The most effective copper(II) complex in this series, 4 , selectivity kills breast CSC‐enriched HMLER‐shEcad cells over breast CSC‐depleted HMLER cells. Furthermore, 4 reduces the formation, size, and viability of mammospheres, to a greater extent than salinomycin, a potassium ionophore known to selectively inhibit CSCs. Mechanistic studies revealed that the CSC‐specificity observed for 4 arises from its ability to generate intracellular reactive oxygen species (ROS) and inhibit cyclooxygenase‐2 (COX‐2), an enzyme that is overexpressed in breast CSCs. The former induces DNA damage, activates JNK and p38 pathways, and leads to apoptosis. 相似文献
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Michal Gacki Karolina Kafarska Wojciech M. Wolf 《Journal of Coordination Chemistry》2019,72(22-24):3481-3494
AbstractA cobalt(II) complex with empirical formula [Co(dicl)2·(H2O)3]·MeOH (where dicl?=?diclofenac) was synthesized and characterized by elemental analysis, flame atomic absorption spectroscopy (FAAS), infrared spectroscopy (FTIR) and thermal decomposition techniques (TGA). The crystal structure of the complex was determined by single crystal X-ray diffraction technique. The compound crystallizes in the monoclinic space group I2/a. Apical water molecules link adjacent cobalt(II) ions forming polymeric chains along the crystal a axis. The thermal behavior of the complex was studied by TG/DTG/DTA, TG/MS and TG/FTIR methods under non-isothermal conditions in air. Upon heating [Co(dicl)2·(H2O)3]·MeOH decomposes progressively to metal oxides, which are the final products of pyrolysis. Furthermore, antioxidant activity of the complex was examined. 相似文献
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Hanan Alatawi Anna Hogan Ibtihaj Albalawi Emma O'Sullivan-Carroll Samia Alsefri Yineng Wang Eric Moore 《Electrophoresis》2022,43(20):1944-1952
A simple, rapid method using CE and microchip electrophoresis with C4D has been developed for the separation of four nonsteroidal anti-inflammatory drugs (NSAIDs) in the environmental sample. The investigated compounds were ibuprofen (IB), ketoprofen (KET), acetylsalicylic acid (ASA), and diclofenac sodium (DIC). In the present study, we applied for the first time microchip electrophoresis with C4D detection to the separation and detection of ASA, IB, DIC, and KET in the wastewater matrix. Under optimum conditions, the four NSAIDs compounds could be well separated in less than 1 min in a BGE composed of 20 mM His/15 mM Tris, pH 8.6, 2 mM hydroxypropyl-beta-cyclodextrin, and 10% methanol (v/v) at a separation voltage of 1000–1200 V. The proposed method showed excellent repeatability, good sensitivity (LODs ranging between 0.156 and 0.6 mg/L), low cost, high sample throughputs, portable instrumentation for mobile deployment, and extremely lower reagent and sample consumption. The developed method was applied to the analysis of pharmaceuticals in wastewater samples with satisfactory recoveries ranging from 62.5% to 118%. 相似文献
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Isobutyric acid in the presence of cyanuric chloride and N‐methylmorpholine was converted into active ester 3 at 0–5 °C, and it was subsequently treated with 3‐aminobenzotrifluoride 4 at 25 °C to furnish corresponding amide 5. This amide finally, on nitration, produced the desired product flutamide, 2‐methyl‐N‐[4‐nitro‐3‐(trifluoromethyl)phenyl]propionamide 6 in good yield. By‐product 2,4,6‐trihydroxy‐1,3,5‐triazine 7 was converted into the useful starting material cyanuric chloride 1 by refluxing with N,N‐diethylamine and POCl3. 相似文献