Past, Present, and Future of Solid Phase Extraction: A Review

Buszewski, Bogusław; Szultka, Małgorzata

doi:10.1080/07373937.2011.645413

Cited by 392 publications

(188 citation statements)

References 130 publications

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“…The protein concentrator and crude sample showed more peaks at retention times before 5 min due to high concentration of inorganic sulfate ( Figure S7). This confirms the need for SPE in sample preparation of target compounds/ analytes, 69,70 as it increases the recovery of the compounds by removing the salts from the reaction buffer by selective isolation/fractionation of the cyclic peptides from the reaction mixture. This is consistent with work carried out by Loroch et al using RP-SPE for phosphopeptide fractionation 71 .…”

Section: Comparison Of Extraction Methodsmentioning

confidence: 73%

Accurate quantification of modified cyclic peptides without the need for authentic standards

et al. 2016

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There is a growing interest in the use of cyclic peptides as therapeutics, but their efficient production is often the bottleneck in taking them forward in the development pipeline. We have recently developed a method to synthesise azole-containing cyclic peptides using enzymes derived from different cyanobactin biosynthetic pathways. Accurate quantification is crucial for calculation of the reaction yield and for the downstream biological testing of the products. In this study, we demonstrate the development and validation of two methods to accurately quantify these compounds in the reaction mixture and after purification. The first method involves the use of a HPLC coupled in parallel to an ESMS and an ICPMS, hence correlating the calculated sulfur content to the amount of cyclic peptide. The second method is an NMR ERETIC method for quantifying the solution concentration of cyclic peptides. These methods make the quantification of new compounds much easier as there is no need for the use of authentic standards when they are not available.

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Section: Comparison Of Extraction Methodsmentioning

confidence: 73%

Accurate quantification of modified cyclic peptides without the need for authentic standards

et al. 2016

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“…24 When SPE in a column format is coupled online with HPLC, a gradient elution is normally used to extract the sample from the SPE column to the analytical one for further LC separation. 25 SPE columns can also be treated as small chromatographic columns with application of gradient elution for sample quantitation 26,27 or to define the breakthrough volumes for optimization of SPE-HPLC experiments. 28 However, when using SPE in direct conjunction with UV, 29 fluorescence, 30 or chemiluminescence 31 detection systems, an isocratic elution is typically employed.…”

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confidence: 99%

Microchip Emitter for Solid-Phase Extraction–Gradient Elution–Mass Spectrometry

et al. 2013

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A microchip electrospray emitter with a magnetic bead trap has been designed for solid-phase extraction-gradient elution-mass spectrometry (SPE-GEMS). The goal of this method is the detection of analytes at low concentrations and it is here demonstrated using reverse phase coated magnetic beads (Mbs) for the preconcentration and detection of the peptides. The sample is passed through the chip, and the peptides are retained and enriched in the trap. After washing, the peptides are released sequentially by stepwise gradient elution and electrosprayed for mass spectrometry analysis. This approach allows effective sample desalting, enrichment, sequential elution, and MS detection without the introduction of an additional separation step after SPE. Efficient preconcentration of model peptides by SPE and sequential release and analysis of peptides by GEMS were demonstrated for diluted sample solutions within the range of 1 μM to 10 nM. Fortified human blood serum, protein digest and fractions collected after protein digest OFFGEL separation were analyzed by SPE-GEMS allowing the detection of low abundance peptides usually not observed by direct mass spectrometry analysis. A mathematical model for gradient elution is proposed.

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“…LLE is based on the equilibrium distribution/partition coefficient between two immiscible liquids. On the other hand, SPE is based on the selective distribution of analytes between the solid packing material and liquid mobile phase [15,16]. The main drawbacks of these two techniques are the important amounts of solvents and the laborious procedures involved.…”

Section: Introductionmentioning

confidence: 99%