Search results for "high-performance liquid chromatography"

Determination of carbosulfan and its metabolites in oranges by liquid chromatography ion-trap triple-stage mass spectrometry.

2005

Liquid chromatography ion-trap mass spectrometry LC-MSn has been successfully applied to identify and confirm carbosulfan and seven of its metabolites in oranges after pressurized liquid extraction (PLE) with dichloromethane. Mass spectra of carbosulfan and its metabolites were investigated using multiple stages of mass spectrometry. Although interpretation of the fragmentation pathways, based on mass spectra, enables structural elucidation and identification of these compounds, the proposed fragmentation pathways and ion structures need verification by exact mass measurements. The analytical method--PLE and LC-MS3 --was validated: limits of quantification (LOQ) ranged from 0.01 to 0.07 mg …

Determination of bisphenol diglycidyl ether residues in canned foods by pressurized liquid extraction and liquid chromatography–tandem mass spectrome…

2005

Abstract A new confirmatory method for simultaneous determination of bisphenol diglycidyl ether residues (BADGE, BADGE·H2O, BADGE·2H2O, BADGE·H2O·HCl, BADGE·HCl, BADGE·2HCl, BFDGE and BFDGE·2HCl) from canned food has been developed. The proposed method includes extraction by pressurized liquid extraction (PLE) followed by liquid–liquid partition and purification by solid phase extraction (SPE). Several solvent systems and different operating conditions (time, temperature) have been investigated for PLE optimization. A reversed-phase high-performance liquid chromatography (RP-HPLC) coupled to atmospheric pressure chemical ionisation tandem mass spectrometry (APCI-MS–MS) method was developed …

Über polygermane

1986

Abstract The synthesis of GePh4 and Ge2Ph6 by Grignard reaction in THF or ether/toluene leads to the by-products Ge3Ph8 (up to 11%) and Ge4Ph10 (up to 18%) which is dependant on using an excess of Mg. A quantitative analysis of the resulting products by HPLC and a semipreparative separation by column, flash, and HPL chromatography is described. The crystal structures of Ge3Ph8 (R = 0.075) and Ge4Ph10 · 2C6H6 (R = 0.054) have been determined. Ge4Ph10 has Ci symmetry and both chain conformations are well staggered (49–70° for Ge3Ph8, 53–66° for Ge4Ph10). The GeGe distances and GeGeGe angles are 244 pm and 121° (Ge3Ph8), and 246 pm and 118° (Ge4Ph10).

BONDED SILICA PHASES FOR THE SEPARATION OF BIOPOLYMERS BY MEANS OF COLUMN LIQUID CHROMATOGRAPHY

1988

Is multidimensional high performance liquid chromatography (HPLC) an alternative in protein analysis to 2D gel electrophoresis?

2000

The interactive modes of High Performance Liquid Chromatography (HPLC) of proteins provide a platform for the construction of a multidimensional HPLC system coupled to mass spectrometry. We present a system composed of both anion and cation exchanger columns, in the first dimension, and n-octadecyl bonded 1.5 μm nonporous silica columns in the second dimension. Both columns are operated under gradient conditions. A system suitability test with standard proteins showed that the total analysis can be performed within about 20 minutes. The fractions taken from the ion exchanger column are directly analyzed within one minute on the reversed phase column at a high flow rate. Two reversed phase c…

Microscale synthesis of phosphatidyl-[3H]choline from 1,2-diacylglycerol. Assessment of isomerization by reversed-phase high-performance liquid chrom…

1995

The synthesis of rac-1-palmitoyl-2-oleoylglycero-3-phospho-[3H]choline of high specific activity was carried out on a microscale by making 7 mumol of rac-1-palmitoyl-2-oleoylglycerol react first with an equimolar amount of POCl3 and then of [3H]choline. After purification by thin-layer chromatography and normal-phase high-performance liquid chromatography and normal-phase high-performance liquid chromatography (HPLC), the yield of the synthesis of [3H]phosphatidylcholine (120 microCi/mumol) was 22%. rac-1-Palmitoyl-2-oleoylglycerol was purified before use by reversed-phase HPLC under conditions which were nonisomerizing and allowed the separation of 1,2- and 1,3-isomers of diacylglycerol. E…

Analysis of eicosapentaenoic and docosahexaenoic acid geometrical isomers formed during fish oil deodorization.

2006

International audience; Addition of long-chain polyunsaturated fatty acids (LC-PUFAs) from marine oil into food products implies preliminary refining procedures of the oil which thermal process affects the integrity of LC-PUFAs. Deodorization, the major step involving high temperatures, is a common process used for the refining of edible fats and oils. The present study evaluates the effect of deodorization temperature on the formation of LC-PUFA geometrical isomers. Chemically isomerized eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) were used as reference samples. Fish oil samples have been deodorized at 180, 220 and 250 °C for 3 h and pure EPA and DHA fatty acid methyl esters…

Performance of short-chain alcohols versus acetonitrile in the surfactant-mediated reversed-phase liquid chromatographic separation of β-blockers

2010

Organic solvents are traditionally added to micellar mobile phases to achieve adequate retention times and peak profiles, in a chromatographic mode which has been called micellar liquid chromatography (MLC). The organic solvent content is limited to preserve the formation of micelles. However, at increasing organic solvent contents, the transition to a situation where micelles do not exist is gradual. Also, there is no reason to neglect the potentiality of mobile phases containing only surfactant monomers instead of micelles (high submicellar chromatography, HSC). This is demonstrated here for the analysis of β-blockers. The performance of four organic solvents (methanol, ethanol, 1-propano…

Review: Determination of Vitamin D in Dairy Products by High Performance Liquid Chromatography

2005

This work reviews the methods used for the determination of vitamin D in some dairy products (milk and infant formulas) by high performance liquid chromatography (HPLC). The low vitamin D contents and the presence of interfering compounds require sample treatment and purification of the extract. The advantages and drawbacks of hot and cold saponification, direct extraction and different types of extract purification are also discussed, taking into account the lack of vitamin D stability by heating, exposure to light and oxidation. With respect to chromatographic determination, the mode (normal or reverse phase), type of column (microcolumn or conventional) and detection system (UV, electro…

Eucalyptol-based green extraction of brown alga Zonaria tournefortii

2018

Abstract A green extraction method, based on the use of 1,8-cineole (eucalyptol) as biosolvent, has been developed to prepare crude extracts from the brown alga Zonaria tournefortii characterized by chemical composition, particularly dominated by phenolic compounds derived from phloroglucinol. The main advantage of the developed technique are the recovery of eucalyptol, based on multistep liquid-liquid extraction with distilled water, followed by centrifugation and elimination of the aqueous phase, and the complete recycling of biosolvent by steam distillation. A comparative study between the proposed green extract and the conventional extract, prepared by solvent maceration using the mixtu…