Analysis of Choline, Carnitine, Acetylcarnitine and Acetylcholine in Animal Feeds, Blood and Urine Using Ion Chromatography Coupled with Tandem Mass Spectrometry

Author(s):  
Suo Decheng ◽  
Fan Xia ◽  
Wei Shulin ◽  
Li Yang

Abstract A simple and sensitive method was proposed for choline, carnitine, acetylcarnitine (ACa) and acetylcholine (ACh) separation in feed, blood and urine of animals by using ion chromatography (IC) and detection by tandem mass spectrometry (MS/MS). Analytes were extracted using a mixture of acetonitrile and water, purified by C18 solid-phase extraction columns, separated via IC with an IonPac SCS-1 column and detected by an MS/MS detector by using isotopic internal standards for quantification. The effects of different chromatographic parameters on the separation were also investigated. Under optimal conditions, the recovery was >90%, with the relative standard deviations of <15%. The proposed method was highly reliable for the simultaneous determination of choline, carnitine, ACa and ACh in feed, blood and urine.

2007 ◽  
Vol 90 (2) ◽  
pp. 604-612 ◽  
Author(s):  
Guy Dufresne ◽  
Andre Fouquet ◽  
Don Forsyth ◽  
Sheryl A Tittlemier

Abstract A multiresidue method was developed to measure low levels of 8 fluoroquinolones (norfloxacin, ofloxacin, danofloxacin, ciprofloxacin, desethylene ciprofloxacin, enrofloxacin, sarafloxacin, and difloxacin) and 4 quinolones (oxolinic acid, flumequine, nalidixic acid, and piromidic acid). Method detection limits range from 0.1 ng/g for quinolones to 0.4 ng/g for fluoroquinolones. Average recoveries range from 57 to 96%, depending on analyte and commodity; relative standard deviations are all less than 18%. The drugs are extracted from tissues using a mixture of ethanol and 1% acetic acid, diluted in aqueous HCl, and defatted by extraction with hexane. The compounds are further isolated using cation-exchange solid-phase extraction and measured using liquid chromatography with electrospray tandem mass spectrometry detection. The method has been evaluated and applied to the analysis of salmon, trout, and shrimp. Detectable residues were observed in 10 out of 73 samples, at concentrations ranging from 0.28 to 16 ng/g.


1994 ◽  
Vol 77 (5) ◽  
pp. 1230-1236 ◽  
Author(s):  
William C Brumley ◽  
Elizabeth M Shafter ◽  
Paul E Tillander

Abstract Eleven phthalate esters spiked in water and soil were determined by tandem mass spectrometry (MS) under positive chemical ionization mass spectrometry (CIMS) conditions with isobutane as reagent gas. Emphasis was placed on the determination step because tandem MS and CIMS are not widely adopted in current methods of the U.S. Environmental Protection Agency. Extraction by sonica-tion and cleanup by use of a solid-phase extraction cartridge were adopted. The relative response factors gave relative standard deviations (RSDs) of 12-30% when 2 unlabeled internal standards were used. The relative abundances of monitored ions gave relative abundance deviations of less than ± 8%. The method confirms identity, including molecular weight, and quantitates with high specificity. Results obtained with 2 unlabeled internal standards were compared with results obtained with a stable-isotope-labeled internal standard for dioctyl phthalate.


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