Search results for "PREP"

Direct determination of Mancozeb by photoacoustic spectrometry

2006

Abstract A solvent free, fast and environmentally friendly photoacoustic-infrared-based methodology (PAS-FTIR) was developed for the determination of Mancozeb in agrochemicals. This methodology was based on the direct measurement of the transmittance spectra of solid samples and a multivariate calibration model to determine the active ingredient concentration. The proposed partial least squares (PLS) model was made using nine standards prepared by mixing different amounts of kaolin and Mancozeb, with concentrations between 5.43 and 88.10% (w/w). A hierarchical cluster analysis was made in order to classify the samples in terms of similarity in the PAS-FTIR spectra. From their spectra differ…

Near-critical carbon dioxide extraction and liquid chromatography determination of UV filters in solid cosmetic samples: A green analytical procedure

2005

Near-critical carbon dioxide extraction of four UV filters used as sunscreens in lipsticks and makeup formulations is reported. Extraction parameters were optimized. Efficient recoveries were obtained after 15 min of dynamic extraction with a 80:20 CO2/ethanol mixture at 300 atm and 54 degrees C, using a 1.8 mL/min flow rate. Extracts were collected in ethanol, and appropriately diluted with ethanol and 1% acetic acid to obtain a 70:30 v/v ethanol/1% acetic acid solution. The four UV filters were determined by LC with gradient elution using ethanol/1% acetic acid as mobile phase. The accuracy of the analytical procedure was estimated by comparing the results with those obtained by methods b…

Extraction of clenbuterol from calf urine using a molecularly imprinted polymer followed by quantitation by high-performance liquid chromatography wi…

2002

A method for the extraction of clenbuterol from calf urine samples using a molecularly imprinted polymer (MIP) has been developed. The aim was that the final extracts from the MIP should allow quantitation of clenbuterol down to 0.5 ng/mL urine using HPLC with UV detection. The MIP was produced using brombuterol as a template and the selectivity of the MIP, for clenbuterol, was tested against a non-imprinted polymer (produced without template) and was found to be high. After loading of 5 mL diluted centrifuged urine, selective binding was established in acetonitrile-acetic acid (98:2). For further elution of interferences, 0.5 M ammonium acetate buffer pH 5 and 70% acetonitrile in water was…

Microwave-assisted extraction of polybrominated diphenyl ethers and polychlorinated naphthalenes concentrated on semipermeable membrane devices

2006

Abstract Microwave-assisted extraction (MAE) has been evaluated as an alternative to dialysis for the extraction of polybrominated diphenyl ethers (PBDEs) and polychlorinated naphthalenes (PCNs) sampled by semipermeable membrane devices (SPMDs), using gas chromatography coupled to tandem mass spectrometry (GC–MS–MS). For MAE optimization a two level full factorial design 2 3 , plus a centre point, which involves 11 randomized runs was used. The results showed that the temperature had a significant influence on the extraction of the nine PBDEs and four PCNs tested. Also, the solvent volume had a positive influence on the extraction of PBDEs and PCNs, but only in latter compounds, it achieves…

Determination of tetracyclines in multi-specie animal tissues by pressurized liquid extraction and liquid chromatography–tandem mass spectrometry

2009

Abstract A specific, sensitive and robust pressurized liquid extraction (PLE) and liquid chromatography tandem mass spectrometry (LC–MS/MS) method for determining tetracycline, chlortetracycline, oxytetracycline and doxycycline in bovine, swine, poultry and lamb muscle tissues is presented. PLE was performed using an ASE ® 200 from Dionex and water as extractant, followed by solid-phase extraction (SPE) using an Oasis HLB cartridge. The method was validated for beef, chicken, pork and lamb meat in compliance with the requirements set by Commission Decision, 2002/657/EC [Commission Decision 2002/657/EC (2002). Implementing Council Directive 96/23/EC concerning the performance of analytical m…

Advanced Sample Preparation Techniques for MS Analysis

2015

Profiling of endogenous peptides by multidimensional liquid chromatography: On-line automated sample cleanup for biomarker discovery in human urine.

2009

A simple and flexible system, employing a column switching technique, has been designed to allow the analysis of peptides and proteins smaller than 15 kDa by molecular weight in filtered urine samples by performing a direct on-column injection utilising simultaneous sample clean-up and trace enrichment. The positively charged peptides and small proteins in the sample are attracted to the inner, negatively charged pore structure of the RAM-SCX column while the larger proteins and uncharged or negatively charged compounds are excluded. After preconditioning with the biological sample, large amounts of sample can be injected. Several important and adjustable parameters for the proper use of a …

Comparison of liquid chromatography using triple quadrupole and quadrupole ion trap mass analyzers to determine pesticide residues in oranges.

2005

Liquid chromatography-triple quadrupole/mass spectrometry (LC-TQ/MS) and liquid chromatography-quadrupole ion trap/mass spectrometry (LC-QIT/MS) for determining bupirimate, hexaflumuron, tebufenpyrad, buprofezin, pyriproxyfen, and fluvalinate in fruits have been compared. The differences in the mass spectra obtained by triple and ion trap quadrupoles are discussed, showing how both of them provide interesting features. The evaluation of the two instruments was carried out by ethyl acetate extraction of oranges spiked with the studied pesticides at LOQ and 10 times the LOQ. Results obtained by LC-TQ/MS correlated well with those obtained by LC-QIT/MS. Recoveries were 70-94% by LC-TQ/MS and 7…

Liquid chromatographic determination of aliphatic amines in water using solid support assisted derivatization with 9-fluorenylmethyl chloroformate

2002

A simple and sensitive method has been developed for the liquid chromatographic determination of short-chain aliphatic amines in water. Analytes are retained in solid-phase extraction (SPE) cartridges, and then derivatized by drawing an aliquot of the fluorogeneic reagent 9-fluorenylmethyl chloroformate (FMOC) through the cartridges. After a certain reaction time the derivatives formed are desorbed with acetonitrile. The collected extracts are then chromatographed on a LiChrospher 100 RP18 125 mm×4 mm i.d., 5 μm, column using an acetonitrile-water gradient. The influence of experimental conditions (SPE material, volume of sample, concentration of FMOC, time of reaction and pH) has been inve…

Supercritical fluid extraction of pesticides

1989

The extraction behaviour of 10 μg samples of five pesticides and some related compounds from glass wool with supercritical CO2 has been investigated under several conditions (10 MPa, 20 MPa extraction pressure, 313 K, dry and water saturated CO2). The extraction fluid was decompressed over a line of little columns, filled with 3μ Si60 or RP18, and the amount of deposited material was analyzed by HPLC for each of these columns. Due to the progressive pressure/density reduction along the line, the solubility diminishes and hence the compounds are deposited according to their polarity/vapor pressure earlier or later on the line. Thus extraction and prefractionation of compounds of different po…