scholarly journals Ultrasound-assisted Matrix Solid Phase Dispersion for the HPLC-DAD analysis of amphenicols in shrimps

2015 ◽  
Vol 2 (1) ◽  
Author(s):  
Victoria F. Samanidou ◽  
Evgenia A. Makrygianni

AbstractUltrasound-assisted matrix solid phase dispersive extraction was applied for the selective isolation and clean-up of three amphenicol antibiotics, chloramphenicol (CAP), thiamphenicol (TAP) and florfenicol (FFC) from shrimp. The target antibiotics were separated on a LiChroCART-LiChrospher® 100 RP-18 (5 μm, 250 × 4 mm) analytical column in less than 9 min, with isocratic elution using a mixture of 70% ammonium acetate (0.05 M) and 30% acetonitrile (v/v). Matrix Solid Phase Dispersion protocol was optimized in terms of extraction sorbent and elution solvent. Two polymer based (Oasis and Nexus) sorbents and one silica based (Lichrolut C18) were compared and different elution solvents such as methanol, acetone, acetonitrile and isopropanol were evaluated based on the achieved recovery rates as well as on the cleanup efficiency. The extraction procedure was performed with and without sonication to evaluate the impact of ultrasounds. TAP and FFC were monitored at 234 nm and CAP at 280 nm by a photodiode array detector. The method was validated according to the European Union Decision 2002/657/EC in terms of linearity, selectivity, stability, accuracy, precision and sensitivity. Detection capability values (CCb) were 64.6 μg/kg for TAP and 1046.8 μg/kg for FFC and 63.8 μg/ kg for CAP.

2014 ◽  
Vol 53 (1) ◽  
pp. 189-195 ◽  
Author(s):  
Mahboobeh Manoochehri ◽  
Ali Akbar Asgharinezhad ◽  
Mahdi Safaei

Separations ◽  
2019 ◽  
Vol 6 (2) ◽  
pp. 30
Author(s):  
Maria Celeiro ◽  
Lua Vazquez ◽  
J. Pablo Lamas ◽  
Marlene Vila ◽  
Carmen Garcia-Jares ◽  
...  

A method based on micro-matrix solid-phase dispersion (μ-MSPD) followed by gas-chromatography tandem mass spectrometry (GC–MS/MS) was developed to analyze UV filters in personal care products. It is the first time that MSPD is employed to extract UV filters from cosmetics samples. This technique provides efficient and low-cost extractions, and allows performing extraction and clean-up in one step, which is one of their main advantages. The amount of sample employed was only 0.1 g and the extraction procedure was performed preparing the sample-sorbent column in a glass Pasteur pipette instead of the classic plastic columns in order to avoid plastizicer contamination. Factors affecting the process such as type of sorbent, and amount and type of elution solvent were studied by a factorial design. The method was validated and extended to other families of cosmetic ingredients such as fragrance allergens, preservatives, plasticizers and synthetic musks, including a total of 78 target analytes. Recovery studies in real sample at several concentration levels were also performed. Finally, the green extraction methodology was applied to the analysis of real cosmetic samples of different nature.


2004 ◽  
Vol 87 (5) ◽  
pp. 1173-1178 ◽  
Author(s):  
G William Chase ◽  
Lin Ye ◽  
Vicky C Stoakes ◽  
Ronald R Eitenmiller ◽  
Austin R Long

Abstract An interlaboratory-verified, liquid chromatographic (LC) method is presented for determination of all-racemic α-tocopheryl acetate and retinyl palmitate in infant formula. The extraction procedure uses matrix solid-phase dispersion. A sample is mixed with C18, and the mixture is packed into a reservoir and eluted with selective solvents to extract the analytes. After evaporation and filtration, the sample extract is injected directly into a normal-phase LC system with fluorescence detection. All-racemic α-tocopheryl acetate and retinyl palmitate are quantitated isocratically with a mobile phase of hexane containing isopropanol at 0.2% (v/v) and 0.125% (v/v), respectively. A nonfortified zero control reference material (ZRM) was spiked at 5 levels, with 5 replicate analyses of 1/2x, x, 2x, 4x, and 16x where “x” represents the minimum levels of 250 IU/100 kcal (vitamin A) and 0.7 IU/100 kcal (vitamin E) as specified in Title 21 of the Code of Federal Regulations, part 107.100. Recoveries of retinyl palmitate ranged from 83.8 to 107%, and those of all-racemic α-tocopheryl acetate ranged from 87.7 to 108%. Two additional laboratories analyzed the ZRM samples at 4 spiking levels with 6 replicates. Recoveries of retinyl palmitate and all-racemic α-tocopheryl acetate ranged from 92.2 to 104% and from 91.7 to 101%, respectively, in the second laboratory. Recoveries of retinyl palmitate and all-racemic α-tocopheryl acetate ranged from 85.3 to 97.0% and from 86.6 to 110%, respectively, in the third laboratory. Relative standard deviations for all 3 laboratories ranged from 0.2 to 7.5% with an average of 2.9%. In addition, each laboratory analyzed a commercial milk- and commercial soy-based infant formula. Excellent agreement in results was obtained between the 3 laboratories for vitamins A and E in all matrixes.


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