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Rapid ultrasound‐assisted dispersive solid‐phase extraction of nonsteroidal anti‐inflammatory drugs in urine using oleic acid functionalized magnetic graphene oxide
Author(s) -
Seidi Shahram,
Moosavi Negar Sabahi,
Shanehsaz Maryam,
Abdolhosseini Marzieh,
Sadeghi Seyed Jamal
Publication year - 2018
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201800663
Subject(s) - chromatography , solid phase extraction , sorbent , extraction (chemistry) , naproxen , chemistry , mefenamic acid , detection limit , central composite design , adsorption , response surface methodology , medicine , alternative medicine , organic chemistry , pathology
Abstract We describe an ultrasound‐assisted magnetic dispersive solid‐phase extraction based on oleic acid functionalized magnetic graphene oxide followed by high‐performance liquid chromatography with ultraviolet detection. The method was applied for the simultaneous determination of ibuprofen, diclofenac, naproxen, and mefenamic acid in urine. The application of sonication led to the good dispersion of the sorbent, and consequently, significant shortened the extraction time. The sorbent was successfully characterized by different techniques. The influence of the adsorption parameters was optimized using a rotational central composite design. In order to improve desorption efficiency, parameters such as type and volume of the eluent and sonication time were investigated and optimized through a one variable at a time method. Under the optimum conditions, limits of detection and precision were between 3.0–25 ng/mL ( n  = 5) and 3.2–7.1%, respectively. The preconcentration factors were found to be 74 for naproxen, 76 for diclofenac, 80 for ibuprofen, and 66 for mefenamic acid corresponding to the absolute recovery within the range of 82.5–100%. Finally, the proposed method was successfully applied for simultaneous determination of target analytes in human urine samples. The relative recovery was within the range of 91.4–113.3%, indicating the good reliability and accuracy of the method.

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