scholarly journals An Accurate Assessment of Docosahexaenoic Acid in Laying Hen Serum for Regulatory Studies

2018 ◽  
Vol 13 ◽  
pp. 117739011881514
Author(s):  
Gerald Patrick Dillon ◽  
Geoff Wallace ◽  
Alexandros Yiannikouris ◽  
Colm Anthony Moran
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Docosahexaenoic Acid ◽  
Tandem Mass Spectrometry ◽  
Electrospray Ionization ◽  
Laying Hen ◽  
Tandem Mass ◽  
Limit Of Quantitation ◽  
Fit For Purpose

Diets rich in omega-3 fatty acids (n-3 FA) have been associated with several health benefits. With the increased interest in n-3 FA both scientifically and societally, the accurate detection of such analytes has become increasingly important. Recently, tandem mass spectrometry (MS/MS) with electrospray ionization interface (ESI), hyphenated to both gas chromatography (GC) and liquid chromatography (LC), has become a valuable tool in the detection of docosahexaenoic acid (DHA). Liquid chromatography-electrospray ionization interface-tandem mass spectrometry methods have been developed for the determination of DHA in canine and poultry species. The objective of this article is to investigate whether LC-ESI-MS/MS is fit for purpose for the determination of DHA in laying hen serum. The disclosure of this work will be beneficial for researchers investigating poultry enrichment for regulatory and toxicological studies. The method was found to be linear over the range. Precision and accuracy results met acceptance criteria and the Limit of Quantitation (LOQ) was established as 1 µg/mL. Recoveries of DHA were obtained for quality control samples and stability studies were performed. The results of the verification study complimented those of the validation study. In summation, the method was established as fit for purpose for measuring total DHA in laying hen serum.

scholarly journals Determination of Deltamethrin Residues in Plant Materials by Liquid Chromatography/Tandem Mass Spectrometry with Electrospray Ionization

2006 ◽  
Vol 89 (3) ◽  
pp. 786-796 ◽  
Author(s):  
Dieter Zimmer ◽  
Christiane Philipowski ◽  
Birgit Posner ◽  
Agnes Gnielka ◽  
Edgar Dirr ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Electrospray Ionization ◽  
Tandem Mass ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Abstract This paper describes a selective and sensitive method that uses liquid chromatography/tandem mass spectrometry with positive electrospray ionization (ESI+) for the determination of deltamethrin in a variety of crops. Samples were extracted by conventional high-speed blending. Some samples required no further cleanup; others were cleaned up by gel permeation chromatography, strong cation-exchange cartridges, or partitioning with n-hexane. In the determinative step, the buffered neutral mobile phase, consisting of 10 mM ammonium acetate (pH 6.8) and methanol, and ESI+ provided strong ammonium adduct formation to [M+NH4]+ at m/z 523, and the multiple-reaction monitoring (MRM) transition at m/z 523/281 was used for the quantitation of deltamethrin. A second MRM transition at m/z 525/283 was used for confirmation. The limit of quantitation (LOQ) values were 0.01 mg/kg for edible materials and 0.05 mg/kg for nonedible materials. Mean overall recoveries at the LOQ and the 10-fold LOQ ranged from 73 to 96%, and the relative standard deviations were <10% for all samples materials analyzed.

scholarly journals Determination of Clenbuterol, Salbutamol, and Cimaterol in Bovine Retina by Electrospray Ionization–Liquid Chromatography–Tandem Mass Spectrometry

2004 ◽  
Vol 87 (1) ◽  
pp. 31-38 ◽  
Author(s):  
Joseph H W Lau ◽  
Cheang S Khoo ◽  
John E Murby
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Electrospray Ionization ◽  
Tandem Mass ◽  
Bovine Retina ◽  
Chromatography Tandem Mass Spectrometry ◽  
Protease Enzyme ◽  
Liquid Chromatography Tandem Mass

Abstract An electrospray ionization–liquid chromatography–tandem mass spectrometry (ESI/LC/MS/MS) method was developed for the simultaneous determination of the β-agonists clenbuterol, salbutamol, and cimaterol in bovine retina. The tissue was homogenized in alkaline buffer and spiked to give 10, 15, and 20 ng/g each of the 3 analytes together with the internal standards d6-salbutamol and d6-clenbuterol. The mixture was incubated with protease enzyme to release any protein-bound analytes and then made alkaline before extraction with isobutanol. The extract was dissolved in water and transferred to a clenbuterol immunoaffinity column. After washing, the analytes were eluted and analyzed by ESI/LC/MS/MS using a C18 column with acetic acid–methanol as mobile phase. No interferences were observed from the spiked retina extract at the various single-reaction monitoring modes. Average recoveries for clenbuterol, salbutamol, and cimaterol were 94, 85, and 87% with coefficients of variation (CVs) of 9.4, 9.9, and 8.6%, respectively. A correlation coefficient of r2 = 0.9999 was obtained for all analytes. The limits of detection for clenbuterol, salbutamol, and cimaterol, determined from 3 times the standard deviation of 7 replicates of the lowest spike, were 2.5, 3.5, and 2.0 ng/g with CVs of 8.9, 11.6, and 7.2%, respectively.

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