Determination of Ticarcillin and Clavulanic Acid in Serum by Liquid Chromatography

1992 ◽  
Vol 75 (1) ◽  
pp. 30-33 ◽  
Author(s):  
Jennifer C Wright ◽  
Carl N Durham ◽  
Jacob R Dunbar

Abstract A liquid chromatographic (LC) method using solidphase extraction for the determination of clavulanic acid and ticarcillin in human serum has been developed. Clavulanic acid and ticarcillin were extracted separately from 1 mL serum using C18 solid-phase extraction cartridges. Eluates were analyzed by the same reversed-phase LC system. The overall mean recovery of clavulanic acid from serum was 99.7 ±2.3%; the lowest level validated in serum was 0.5 μg/mL. The overall mean recovery of ticarcillin from serum was 101.5 ±3%; the lowest level validated in serum was 12.5 μg/mL. Detection limits for clavulanic acid and ticarcillin were 0.117 and 0.749 μg/mL, respectively.

2005 ◽  
Vol 88 (3) ◽  
pp. 679-683 ◽  
Author(s):  
Matthew J Gramse ◽  
Paul E Jacobson

Abstract A liquid chromatographic method was developed for the determination of penicillin G in feeds. The method involves extraction of penicillin G with methanol, concentration under a stream of nitrogen, and cleanup using Phenomenex Strata-X solid-phase extraction cartridge. Analyte separation and quantification were achieved by gradient reversed-phase liquid chromatography and ultraviolet absorbance at 230 nm. Average spike recoveries for samples prepared at 3 spiking levels (25, 50, and 200 g/ton) were 96.3, 92.1, and 88.6%, respectively. The overall method precision at each of the 3 spiking levels was ≤5.39% relative standard deviation. The limits of detection and quantititation (g/ton formulation) were 3.89 and 13.0 g/ton, respectively.


2004 ◽  
Vol 87 (4) ◽  
pp. 937-942 ◽  
Author(s):  
Harumi Oshima ◽  
Eiji Ueno ◽  
Isao Saito ◽  
Hiroshi Matsumoto

Abstract A simple solid-phase extraction (SPE) method was developed for the liquid chromatography (LC) determination of pheophorbide (Phor) a and pyropheophorbide (Pyro) a in health foods such as chlorella, spirulina, etc. The food sample was extracted with 85% (v/v) acetone. The extract was acidified with hydrochloric acid and loaded on a C18 cartridge. After washing with water, Phor a and Pyro a were eluted with the LC mobile phase. Phor a and Pyro a were separated by isocratic reversed-phase LC and quantitated by fluorescence detection. The recoveries for spiked samples of chlorella and the extract were 87.1–102.0%. Commercial health foods (chlorella, spirulina, aloe, kale, Jews mallow, and green tea leaves) were analyzed using the SPE method. The values found for Phor a and Pyro a ranged from 2 to 788 μg/g and from <1 to 24 μg/g, respectively. There was no significant difference between the SPE method and the official method in Japan (spectrophotometry after liquid–liquid extraction). The advantages of the SPE method are the short extraction times, lack of emulsions, and reduced consumption of organic solvents compared with the official method in Japan. The SPE method is considered to be useful for the screening of Phor a and Pyro a in health foods.


1999 ◽  
Vol 82 (6) ◽  
pp. 1345-1352 ◽  
Author(s):  
Lambert K Sørensen ◽  
Heļga Hansen ◽  
Lena Snor

Abstract A liquid chromatographic (LC) method based on solid-phase extraction was developed for determination of amoxicillin in muscle tissue of rainbow trout. The compound was extracted in an aqueous solution by precipitation of organic material with a mixture of sulfuric acid and sodium tungstate. The extract was processed by solid-phase extraction on an end-capped phenyl sorbent, and concentrated on a divinylbenzene-co-ΛN-vinylpyrrolidone polymeric sorbent. The extract was derivatized and analyzed by reversed-phase gradient LC on a C18 column with UV detection at 323 nm. The method detection limit was 2.9 μg/kg. Mean recovery in muscle was 80.5% (range 10-200 μg/kg). The method was applied to fillets from trout offered feed containing amoxicillin in an aquaculture pilot plant. Amoxicillin was detected in muscle tissue shortly after administration but not 3 weeks later. The relative repeatability standard deviation for incurred residues in muscle tissue was 6.4% (range 11-143 μg/kg).


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