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A simple and rapid dispersive liquid–liquid microextraction method followed by GC‐FID for determination of N ‐methylpyrrolidine in cefepime
Author(s) -
Farajzadeh Mir Ali,
Goushjuii Leila,
Bashour Yousef
Publication year - 2010
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.201000510
Subject(s) - chromatography , chemistry , extraction (chemistry) , flame ionization detector , cefepime , solvent , repeatability , calibration curve , gas chromatography , detection limit , analytical chemistry (journal) , organic chemistry , biochemistry , antibiotic resistance , imipenem , antibiotics
A simple, rapid and efficient sample preparation technique, dispersive liquid–liquid microextraction, coupled with gas chromatography‐flame ionization detection has been developed to determine N ‐methylpyrrolidine in cefepime. The effect of various experimental factors on the preparation procedure, such as the nature and volume of extraction and disperser solvents, extraction time, the nature of buffer and its pH, and salt effect, was investigated, optimized and the following results were obtained: extraction solvent, chloroform; dispersive solvent and solvent for dissolving cefepime, a mixture of methanol/water (88:12, v/v); salting out agent, NaCl; and buffer, carbonate/bicarbonate ( C =0.5 M, pH=12). The optimized conditions were applied to the real sample (cefepime) for the extraction and determination of N ‐methylpyrrolidine. The calibration graph is linear from 0.02 to 850 mg/L with the square of correlation coefficient 0.999. LOD and LOQ are 6.4 and 21.2 μg/L in solution, respectively, and 0.2 (2×10 −5 ) and 0.6 (6×10 −5 ) μg/g (%, w/w) in cefepime powder, respectively, using sample size 50 mg. Repeatability of the method is good and RSD% for six repeated experiments ( C =170 mg/L) is 6.35%.