Sensitive high-performance liquid chromatographic quantitation of gabapentin in human serum using liquid–liquid extraction and pre-column derivatization with 9-fluorenylmethyl chloroformate

2006 ◽  
Vol 835 (1-2) ◽  
pp. 123-126 ◽  
Author(s):  
Gholamreza Bahrami ◽  
Amir Kiani
1999 ◽  
Vol 82 (5) ◽  
pp. 1046-1053 ◽  
Author(s):  
Murielle Juhel-Gaugain ◽  
Béatrice Anger ◽  
Michel Laurentie

Abstract A high-performance liquid chromatographic (HPLC) method for the simultaneous determination of tilmicosin, tylosin, spiramycin, and its major metabolite neospiramycin was developed that is suitable for porcine, bovine, and poultry muscles. Macrolide residues were extracted from muscle with acetonitrile, fat was removed by liquid-liquid extraction with isooctane, and the extract was then cleaned on Bond Elut C18 cartridges. The HPLC separation was performed on an Inertsil ODS3 C18 column (150 × 4 mm) with 0.05% trifluoroacetic acid-acetonitrile in a gradient mode. Two different chromatographic gradients were used for tilmicosin-tylosin and spiramycin-neospiramycin, and the detection wavelengths were 287 and 232 nm, respectively. The method was validated from ½ the maximum residue limit (MRL) to 4 times the MRL with pork muscle samples. Mean recoveries were 60, 63.5, 51, and 42% for tilmicosin, tylosin, spiramycin, and neospiramycin, respectively. The detection limits are 15 μg/kg for tilmicosin and tylosin, 30 μg/kg for spiramycin, and 25 μg/kg for neospiramycin. Linearity, precision, and accuracy of the method were also tested.


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