scholarly journals Optimization of the Matrix Solid Phase Dispersion Extraction Procedure for the Analysis of Polybrominated Diphenyl Ethers in Human Placenta

2009 ◽  
Vol 81 (23) ◽  
pp. 9795-9801 ◽  
Author(s):  
R. M. A. Priyanthi S. Dassanayake ◽  
Hua Wei ◽  
Rachel C. Chen ◽  
An Li
2014 ◽  
Vol 1360 ◽  
pp. 57-65 ◽  
Author(s):  
A. Iparraguirre ◽  
R. Rodil ◽  
J.B. Quintana ◽  
E. Bizkarguenaga ◽  
A. Prieto ◽  
...  

2002 ◽  
Vol 85 (1) ◽  
pp. 128-133 ◽  
Author(s):  
Consuelo Sánchez-Brunete ◽  
Beatriz Albero ◽  
Ester Miguel ◽  
José Luis Tadeo

Abstract A multiresidue method was developed for the determination of 12 organophosphorus insecticides (diazinon, parathion methyl, fenitrothion, pirimiphosmethyl, malathion, fenthion, chlorpyrifos, quinalphos, methidathion, ethion, azinphosmethyl, coumaphos), one carbamate (pirimicarb), and one amidine (amitraz) in unifloral and multifloral honeys. The analytical procedure was based on the matrix solid-phase dispersion of honey on a mixture of Florisil and anhydrous sodium sulfate in small glass columns and subsequent extraction with a low volume of hexane–ethyl acetate (90 + 10, v/v), assisted by sonication. The insecticide residues were determined by capillary chromatography with nitrogen–phosphorus detection and confirmed by mass spectrometry. Average recoveries at the 0.05–0.5 μg/g levels were >80% for organophosphorus insecticides and about 60% for the other insecticides, pirimicarb and amitraz, with relative standard deviations <10%. The detection limit for the different insecticides ranged between 6 and 15 μg/kg. The main advantages of the proposed method are that extraction and cleanup are performed in a single step with a low volume of organic solvent. The method is simple, rapid, and less laborious than conventional methods. Several Spanish honeys were analyzed with the proposed method and no residues of the studied insecticides were found.


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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