scholarly journals Temperature Effects on Retention and Separation of PAHs in Reversed-Phase Liquid Chromatography Using Columns Packed with Fully Porous and Core-Shell Particles

2016 ◽  
Vol 2016 ◽  
pp. 1-12 ◽  
Author(s):  
Christophe Waterlot ◽  
Anaïs Goulas

Effects of temperature on the reversed-phase chromatographic behavior of PAHs were investigated on three columns. The first was the recent C18column (250 mm × 4.6 mm) packed with 5 µm core-shell particles while the others were more conventional C18columns (250 mm × 4.6 mm) packed with fully porous particles. Among the 16 PAHs studied, special attention has been paid to two pairs of PAHs, fluorene/acenaphthene and chrysene/benzo[a]anthracene, which often present coeluting problems. Due to the low surface area of the core-shell particles, lowest retention time of each PAH was highlighted and effects of the temperature on the separation of PAHs were negligible in regard to those using columns packed with fully porous particles. For each PAH studied, it was demonstrated that peaks were symmetrical and may be considered as Gaussian peaks when the column packed with core-shell particle was employed. In the best condition, the separation of PAHs was conducted at 16°C under very low pressure values (670–950 psi = 46–65 bars). Depending on PAHs, the limit of detection ranged from 0.88 to 9.16 μg L−1. Analysis of spiked acetonitrile samples with PAHs at 10 and 50 µg L−1and tap water at 10 µg L−1gave very good recoveries (94%–109.3%) and high precision (1.1%–3.5%).

1995 ◽  
Vol 78 (6) ◽  
pp. 1519-1521 ◽  
Author(s):  
K Bruce Kirksey ◽  
Thomas C Mueller

Abstract Seven extraction methods were examined to determine which one provided a simple, efficient clomazone extraction from aged soil. The method selected involved adding 80 mL acetonitrile to moist soil and shaking for 16 h. The extract was filtered, and an additional 80 mL acetonitrile was added, equilibrated for 1 h, and filtered. Filtrates were combined and concentrated with a rotary evaporator. Clomazone concentrations were then determined by reversed-phase liquid chromatography with UV detection at 220 nm. Recovery with this method was equal to a 16 h + 1 h extraction with methanol, but acetonitrile was selected as extraction solvent because of its ease of removal with a rotary evaporator. The recovery from fortified soil samples was >80%, and a conservative lower limit of detection was 40 ng/g soil.


RSC Advances ◽  
2014 ◽  
Vol 4 (44) ◽  
pp. 22875-22887 ◽  
Author(s):  
Endler M. Borges ◽  
Mauricio A. Rostagno ◽  
M. Angela A. Meireles

The need for increased throughput and superior performance has increased the demand for stationary phases with improved kinetic performance.


1984 ◽  
Vol 30 (11) ◽  
pp. 1789-1791 ◽  
Author(s):  
B G Charles ◽  
P J Ravenscroft

Abstract We describe a rapid, specific, and precise analysis for gliclazide in plasma by radial compression, reversed-phase, "high-performance" liquid chromatography. Gliclazide and the internal standard, 3-chlorogliclazide, are eluted after 4.4 and 6.8 min, respectively. Only 100 microL of plasma and minimal sample workup are required. The limit of detection for gliclazide in plasma is 0.5 mg/L (1.55 mumol/L) at 229 nm. Precision (CV) of the assay for 10 and 1 mg of gliclazide per litre is 2.1% and 6.4%, respectively.


1996 ◽  
Vol 79 (4) ◽  
pp. 839-843 ◽  
Author(s):  
Wenhong Luo ◽  
Eugene B Hansen ◽  
Catharina Y W Ang ◽  
Harold C Thompson

Abstract A method is described for detecting and quantitating lincomycin residue in salmon muscle and skin tissues by ion-pair reversed-phase liquid chromatography (LC) with electrochemical detection at +0.9 V. Lincomycin was extracted from tissues by homogenizing with 0.01 M KH2PO4 buffer (pH 4.5) and centrifuging the mixture. Water-soluble proteins were precipitated by adding sodium tungstate and sulfuric acid and removed by cent r if u gat ion. The buffer extract was then passed through a C18 solid-phase extraction cartridge. Lincomycin was eluted with 50% acetonitrile in water, and the eluate containing lincomycin was extracted with ethyl acetate. After the solvent had evaporated, the residue was redissolved in mobile phase and analyzed by LC. The method had a limit of detection of 7 ng/g lincomycin for salmon muscle and 12 ng/g for salmon skin. The limit of quantitation was 17 ng/g for salmon muscle and 24 ng/g for salmon skin. Average recoveries of lincomycin spiked at 50,100, and 200 ng/g were ≥85% for salmon muscle and ≥80% for salmon skin.


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