scholarly journals Simple and Fast Methods Based on Solid-Phase Extraction Coupled to Liquid Chromatography with UV Detection for the Monitoring of Caffeine in Natural, and Wastewater as Marker of Anthropogenic Impact

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Sònia Moret ◽  
Manuela Hidalgo ◽  
Juan M. Sanchez
Keyword(s):  
Detection Limit ◽  
Solid Phase Extraction ◽  
Natural Waters ◽  
Wastewater Treatment Plants ◽  
Solid Phase ◽  
Sample Volume ◽  
Uv Detection ◽  
Phase Extraction ◽  
Method Detection Limit ◽  
Spe Method

Two concentration methods for fast and routine determination of caffeine (using HPLC-UV detection) in surface, and wastewater are evaluated. Both methods are based on solid-phase extraction (SPE) concentration with octadecyl silica sorbents. A common “offline” SPE procedure shows that quantitative recovery of caffeine is obtained with 2 mL of an elution mixture solvent methanol-water containing at least 60% methanol. The method detection limit is 0.1 μg L−1 when percolating 1 L samples through the cartridge. The development of an “online” SPE method based on a mini-SPE column, containing 100 mg of the same sorbent, directly connected to the HPLC system allows the method detection limit to be decreased to 10 ng L−1 with a sample volume of 100 mL. The “offline” SPE method is applied to the analysis of caffeine in wastewater samples, whereas the “on-line” method is used for analysis in natural waters from streams receiving significant water intakes from local wastewater treatment plants.

scholarly journals Determination of dimethoate, 2,4-dichlorophenoxy acetic acid, mecoprop and linuron pesticides in environmental waters in Republic of Macedonia by high performance liquid chromatography

2008 ◽  
Vol 27 (1) ◽  
pp. 25 ◽  
Author(s):  
Aleksandra Nestorovska-Krsteska ◽  
Meri Mirčeska ◽  
Jean-Jacques Aaron ◽  
Zoran Zdravkovski
Keyword(s):  
Acetic Acid ◽  
Solid Phase Extraction ◽  
High Performance ◽  
Solid Phase ◽  
Sampling Period ◽  
Phase Extraction ◽  
Environmental Waters ◽  
Spe Method ◽  
Dichlorophenoxy Acetic Acid

An HPLC-UVDAD method for determination of dimethoate, 2,4-dichlorophenoxy acetic acid (2,4-D), mecoprop (MCPP) and linuron in environmental waters was developed. The water samples were concentrated and extracted by a solid phase extraction (SPE) method on Bond Elut PPL cartridges. After extraction the investigated compounds were separated on Stability RP Pesticides chromatographic column using mobile phase composed of acetonitrile- water-acetic acid in volume fractions of 39:59:2 and flow rate of 0.7 mL/min. Ultraviolet absorption detection was carried out for dimethoate, 2,4-D and MCPP at 229 nm, and for linuron at 249 nm. Recoveries made from 500 mL of drinking waters using solid phase extraction ranged between 64.3–92.1 %. The method was applied to environmental waters in Macedonia that receive runoffs from agriculture lands. The levels of pesticides under study ranged between 0.31 μg/L and 7.05 μg/L, depending on the compound and sampling period.

scholarly journals Preconcentration of Copper with Solid Phase Extraction and its Determination by Flame Atomic Absorption Spectrometry

2008 ◽  
Vol 5 (4) ◽  
pp. 878-883 ◽  
Author(s):  
Ayob Parchehbaf Jadid ◽  
Habibollah Eskandari
Keyword(s):  
Detection Limit ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Copper Ions ◽  
Absorption Spectrometry ◽  
Phase Extraction ◽  
Flame Atomic Absorption ◽  
Low Levels ◽  
Determination Of Copper

A new method for the solid phase extraction (SPE) and determination of copper ions at low levels is presented. Extraction percent and the effects of some factors were evaluated. The detection limit was in the range of 2.26 µg·L-1. This procedure has been successfully applied to determination of copper in water samples.

scholarly journals Determination of Flumorph Residues in Vegetables, Soil, and Natural Water by Solid-Phase Extraction Cleanup and High-Performance Liquid Chromatography with UV Detection

2008 ◽  
Vol 91 (6) ◽  
pp. 1459-1466 ◽  
Author(s):  
Ji-Ye Hu ◽  
Yu-Chao Zhang ◽  
Hai Yan
Keyword(s):  
Solid Phase Extraction ◽  
Natural Water ◽  
High Performance ◽  
Solid Phase ◽  
Residue Analysis ◽  
Reversed Phase ◽  
Uv Detection ◽  
Phase Extraction ◽  
Limit Of Quantification

Abstract A method for high-performance liquid chromatographic (HPLC) determination of flumorph residues in cucumber, tomato, soil, and natural water was developed and validated. Primary secondary amine or octadecylsilyl (C18) solid-phase extraction cartridges were used for sample preparation. Reversed-phase HPLC with UV detection was used for separation and quantification of the pesticide. The combined cleanup and chromatographic method steps were sensitive and reliable for simultaneous determination of residues of the 2 isomers of flumorph in the studied samples. This method is characterized by recovery >97.9, coefficient of variation <6.2, and limit of quantification of 0.01 mg/kg, in agreement with directives for method validation in residue analysis. Flumorph residues in the samples were further confirmed by HPLC/mass spectrometry. The proposed method is fast, easy to perform, and could be used for monitoring of pesticide residues.

scholarly journals Development of a Solid-Phase Extraction Method for Determination of Pheophorbide a and Pyropheophorbide a in Health Foods by Liquid Chromatography

2004 ◽  
Vol 87 (4) ◽  
pp. 937-942 ◽  
Author(s):  
Harumi Oshima ◽  
Eiji Ueno ◽  
Isao Saito ◽  
Hiroshi Matsumoto
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Reversed Phase ◽  
Official Method ◽  
Phase Extraction ◽  
Pheophorbide A ◽  
Significant Difference ◽  
Spe Method

Abstract A simple solid-phase extraction (SPE) method was developed for the liquid chromatography (LC) determination of pheophorbide (Phor) a and pyropheophorbide (Pyro) a in health foods such as chlorella, spirulina, etc. The food sample was extracted with 85% (v/v) acetone. The extract was acidified with hydrochloric acid and loaded on a C18 cartridge. After washing with water, Phor a and Pyro a were eluted with the LC mobile phase. Phor a and Pyro a were separated by isocratic reversed-phase LC and quantitated by fluorescence detection. The recoveries for spiked samples of chlorella and the extract were 87.1–102.0%. Commercial health foods (chlorella, spirulina, aloe, kale, Jews mallow, and green tea leaves) were analyzed using the SPE method. The values found for Phor a and Pyro a ranged from 2 to 788 μg/g and from <1 to 24 μg/g, respectively. There was no significant difference between the SPE method and the official method in Japan (spectrophotometry after liquid–liquid extraction). The advantages of the SPE method are the short extraction times, lack of emulsions, and reduced consumption of organic solvents compared with the official method in Japan. The SPE method is considered to be useful for the screening of Phor a and Pyro a in health foods.

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