Part No: IST1072SIssued year: 2006File size: 0.03mbFile type: pdf
This method describes the extraction of quaternary amines, strongly basic amines and amines that are unstable at high pH levels, from biological fluids. The mechanism is mixedmode
hydrophobic and weak cation exchange, allowing acidic elution conditions.
Part No: AN-IST1004SIssued year: 2008File size: 0.04mbFile type: pdf
This method describes a procedure for the determination of Total Oil and Grease using IR as the technique for final analysis. This represents recommendations for SPE method development. The proposed steps are based on experience with similar analytes and matrices, but have not been verified in Biotage laboratories. Please refer to section below for the analyte and matrix considerations that were made in developing this method. As for all method development, this procedure should first be developed using pure solvent spiked with analyte. Only after the chemistry is established should spiked matrix samples be tested.
Part No: AN-IST1009SIssued year: 2008File size: 0.04mbFile type: pdf
This method describes the use of a strong cation exchange SPE column for the extraction of pyridoxine, riboflavin and thiamine from biological fluid samples. This represents recommendations for SPE method development. The proposed steps are based on experience with similar analytes and matrices, but have not been verified in Biotage laboratories. Please refer to section below for the analyte and matrix considerations that were made in developing this method. As for all method development, this procedure should first be developed using pure solvent spiked with analyte. Only after the chemistry is established should spiked matrix samples be tested.
Part No: PPS347Issued year: 2014File size: 0.49mbFile type: pdf
Trends on chemical synthesis have changed over recent years, with a more targeted approach to molecular design becoming more prevalent. As a result, the speed with which a new compound can be synthesized is key to an efficient laboratory.
Part No: TN522Issued year: 2004File size: 0.03mbFile type: pdf
Microwave assisted organic synthesis has become an important tool to medicinal chemists for rapid organic synthesis. Thousands of research papers have appeared over the last decades on the application of microwave technology in organic synthesis.1 Some of the major advantages include a spectacular decrease in reaction time, improved conversions, clean product formation and wide scope for the development of new reaction conditions.
Part No: Issued year: 2002File size: 0.36mbFile type: pdf
The first decision that needs to be made is what the final analysis will be for the analyte. This will have an impact on the sample and cartridge size, as well as the final elution solvent. Gas chromatography offers higher sensitivity than HPLC, while HPLC is better suited for ionisable species and very high molecular weights. If LC-MS is available, minimal sample clean-up may be required.
Part No: P021Issued year: 2008File size: 1.87mbFile type: pdf
It is well known that traditional liquid-liquid extraction (LLE) provides very clean extracts prior to LC/MS analysis. Supported liquid extraction is analogous to traditional LLE, however, analyte partitioning takes place using an inert support material, rather than two immiscible liquids. This provides excellent extraction efficiencies while alleviating
many of the tedious liquid handling issues associated with LLE.
1) Remember to add stir bar for efficient mixing. Catalysts, salts, or visible precipitate should be washed clear of head space and into solution. Particles adhering to glass head space could cause excessive heating increasing possibility of failure of vial. Stay within specified vial volume range (see diagram for proper filling).
Part No: P080Issued year: 2014File size: 0.88mbFile type: pdf
This poster describes the benefits of supported liquid extraction and highlights its use in removal of endogenous matrix components that cause ion suppression/enhancement (matrix effects) in LC-MS/MS analyses.
Part No: P118Issued year: 2015File size: 0.48mbFile type: pdf
This poster examines the use of ISOLUTE SLE+ columns as an alternative to SPE for the extraction and clean up of hair samples containing drugs of abuse. SLE was found to be a simple, faster alternative to SPE for this type of analysis.
Part No: P089Issued year: 2014File size: 0.79mbFile type: pdf
This poster presents a novel method for the simultaneous extraction, derivatization and subsequent detection of both the traditional 25-hydroxy and the biologically active 1α,25-dihydroxy vitamin D metabolites in serum.
Part No: Issued year: 2013File size: 0.35mbFile type: pdf
Leu-Enkephalin-amide (YGGFLNH2, Ca. MW = 554.65) was synthesized on the Rink amide ChemMatrix® resin at a scale of 0.5 mmol. Crude peptide (100 mg) was purified in duplicate using the Isolera Dalton equipped with a Biotage® SNAP KP-C18-HS 12g cartridge.
Part No: AN097Issued year: 2014File size: 0.73mbFile type: pdf
A branched peptidoglycan mimic and a tetra-branched antimicrobial peptide analogue were synthesized on a lysine scaffold using Biotage® Initiator+ Alstra™ microwave peptide synthesizer. These peptide modifications are challenging to synthesize and automate, however, the procedure was operationally simplified using Branches™.
Part No: AN053Issued year: 2010File size: 0.92mbFile type: pdf
It has recently been demonstrated that specific recognition of rhizobial bacteria by the signaling molecule Nod-factor receptor 5 (NFR5) relies on LysM domains. The LysM (lysine motif) domain is believed to be involved in the regulation of the interaction between plants and rhizobial bacteria to promote plant growth. The LysM domain is predicted to consist of two-α
helices and a two-stranded anti-parallel β-sheet in a β-α-α-β structure and has been identified in NFR5 by sequence alignment of the crystal structure with the LysM domain of Bacillus subtilis ykuD.2 The synthesis of the C-terminal and the N-terminal regions of LysM domains provide significant challenges, this is presumably due to the formation of β-sheet like structures, which are known to pose problems for peptide chain assembly.
Part No: AN055Issued year: 2012File size: 0.28mbFile type: pdf
C-terminal peptide aldehydes are key components in oxime and hydrazine ligations and their synthesis is therefore very desirable. A well established method for the synthesis of C-terminal modified peptides including peptide aldehydes, is the backbone amide linker (BAL) strategy (Scheme 1).1 In this strategy, the first amino acid is anchored by reductive amination followed by acylation of the newly formed secondary amine. Thus, the growing peptide chain is anchored not through the C-terminal carboxyl but through a backbone amide nitrogen giving access to, in principle, any C-terminal modification.
Part No: AN054Issued year: 2011File size: 0.39mbFile type: pdf
A number of biologically active natural products contain N-methyl amino acids. N-Methyl amino acid containing peptides are potentially useful therapeutics as they have improved pharmacological properties such as such as proteolytic stability, bioavailability, lipophilicity, enhanced potency and receptor selectivity. The synthetic challenges associated with the synthesis of peptides containing consecutive N-methyl amino acids are well known1,2 and often require coupling reagents such as PyBOP3, HATU4 or even triphosgene4 to obtain high coupling yields. Syro Wave.
Part No: AN052Issued year: 2010File size: 0.26mbFile type: pdf
One of the current challenges in peptide science is the assembly of long peptides and small proteins, which has to overcome the accumulation of side-reactions and the hurdles posed by so-called difficult sequences. During the synthesis of difficult sequences the peptide chain most likely becomes partially inaccessible typically due to the formation of secondary structures, especially β-sheets, which can inhibit acylation and deprotection during synthesis, resulting in truncated sequences. In addition, steric hindrance from β-branched amino acids can be a problem.
Part No: Issued year: 2014File size: 1.01mbFile type: pdf
We have demonstrated the capability of the Biotage® Initiator+ Alstra
microwave peptide synthesizer to fully synthesize branched and cyclic
peptides. The synthesis included specialized reactions of non-linear peptides and a high degree of purity was achieved. Furthermore, the Branches software feature provides an extensive overview for the scheduling and visualization of operations in order to make complex peptide modifications and is a great addition to the toolbox for the peptide chemist. Presented at EPS, Sofia, 2014.
Part No: Issued year: 2005File size: 0.29mbFile type: pdf
Microwave technology at ChemDiv
Standard procedure for Suzuki coupling:
Building block 1-25 (0.25 mmol), the correspondent boronic acid (0.50 mmol) was heated under microwave irradiation (180oC, 10-40 min) in the presence of catalyst [PdCl2(PPh3)2 or dichlorobis(triphenyl-phosphine)palladium(II) polymer bound and Cs2CO3 as a base in DME/Water (50/50) as solvent.
Part No: AN081Issued year: 2014File size: 0.79mbFile type: pdf
This application demonstrates the reproducible multiple peptide
synthesis on a Syro parallel peptide synthesizer equipped with Syro
heating blocks. Effective heat transfer combined with efficient vortex
mixing make this system a powerful tool for the synthesis of multiple
peptides with increased throughput capability.
Part No: AN069Issued year: 2013File size: 0.47mbFile type: pdf
The human β-amyloid (1-42), H-DAEFRHDSGYEVHHQKLVFFAEDVGSNKGAIIGLMVGGVVIA-NH2 (1), sequence is a wellknown difficult sequence to synthesize.1,2 This is due to its
high hydrophobicity at the C-terminus and on-resin aggregation. The peptide is known to be one of the main constituents in amyloid plaques in the brain of Alzheimer’s patients.
Synthetic amyloid peptides are essential research tools to study the molecular mechanisms of neurodegenerative diseases, however, their solid-phase assembly is non-trivial.
Part No: TN/UG-0029.0110Issued year: 2009File size: 0.75mbFile type: pdf
The Biotage Syro Wave™ system is a programmable peptide synthesizer that is capable of both conventional room temperature parallel peptide synthesis and microwave assisted peptide synthesis. The system is a fully automated and computer controlled peptide
synthesizer, based on a pipetting robot with a single arm.
Part No: Issued year: 2011File size: 0.23mbFile type: pdf
• Biologically active peptides isolated from natural sources, e.g. marine sponges, often contain multiple N-methylated residues. Additionally, Nmethylation of synthetic peptides can improve pharmacokinetic properties like bio-availability and stability.
Part No: Issued year: 2006File size: 0.09mbFile type: pdf
Why Use MAOS?
• Accelerated reaction kinetics
• Increased conversion of starting materials to products
• Reaction mixtures are often cleaner than conventional synthesis
• Small to large scalability
• Auto-sampler allows for overnight runs
• Extremely easy to operate
Part No: Issued year: 2010File size: 1.9mbFile type: pdf
User Report: V-10, Sumitomo Dainippon Pharma. Sumitomo Dainippon Pharma is recognized worldwide for its highly creative drug discovery program for treating neuropsychiatric disorders, and in specialized areas with high unmet medical needs. Its Genomic Science Laboratories installed the V-10 evaporation system in 2008, which has been used extensively for drying in-house compounds. We asked two researchers at that facility, Mr. Masahiko Ikeda and Mr. Fumitaka Nishino, about their use of the V-10 in their daily work.
Part No: Issued year: 2005File size: 0.57mbFile type: pdf
Use of the unique opportunities of an academic environment for the synthesis of high-quality libraries of diverse chemical structures to discover small molecules with
architecturally novel scaffolds and a wide range of physicochemical properties and to develop innovative new methodologies for Diversity-Oriented Organic Synthesis
Part No: TN115Issued year: 2006File size: 0.08mbFile type: pdf
This Chemistry Data Sheet describes the use of ISOLUTE® HM-N as a support material for pre-absorption of a
reaction mixture prior to flash chromatography. This approach is used as a solution to loading reaction
mixtures that are only soluble in polar solvents onto an ISOLUTE Flash SI II or Flash NH2 column.
Part No: TN118Issued year: 2006File size: 0.07mbFile type: pdf
ISOLUTE HM-N is a modified form of diatomaceous earth that can efficiently absorb aqueous samples. ISOLUTE HM_N is chemically inert and stable in the pH range 1-13. These characteristics make it a versabile material that plays an important role in many sample preparation applications.
Part No: Issued year: 2006File size: 0.83mbFile type: pdf
• Novo Nordisk A/S & radiochemistry at Novo Nordisk A/S
• Introduction to radiochemistry in general
• Radiochemistry & microwaves
• Selected case stories from the labs at Novo Nordisk A/S
• Applications of radiolabelled compounds
• Summary and acknowledgements
Part No: P016Issued year: 2007File size: 0.16mbFile type: pdf
In order to obtain a fast synthesis of an N-unprotected tripeptide, microwave (mw) assisted deprotection, coupling and partial deprotection were applied starting with a purified protected dipeptide [Fig. 1]. The three consecutive mw assisted steps were performed without any intermediate purifications and were accomplished within some 30 minutes. The resulting crude mixture containing the Boc deprotected tripeptide ester was shown to be quite complex [Fig. 2]. The crude product was subjected to automated reversed phase flash chromatography, followed by automated fraction pooling and “thin film evaporation”. The total time for the entire procedure was 1 h 20 min. The purity of the product was > 99%.
Part No: CM-TRIT-0810Issued year: 2010File size: 0.26mbFile type: pdf
Trityl-ChemMatrix is mainly used to obtain a protected peptide as is has very low TFA cleavage conditions (under 1%). This resin therefore has the same cleavage conditions as the Cl-Trityl-polystyrene. On request, Trityl-ChemMatrix resins can
be offered preloaded will all 20 natural amino acids. Other amino acids can be preloaded on special request. Please take note that the Cl-Trityl-ChemMatrix resin is not offered for stability reasons. It is most effective to start with the Trityl-
OH-ChemMatrix resinchlorinate the resin and then add the amino acid of desire.
Part No: UI324Issued year: 2015File size: 0.75mbFile type: pdf
In determining the gas flow rate, the goal is to achieve
the maximum evaporation rate possible without
splashing or compromising the sample. During
evaporation the distance between the nozzle tips
and the liquid surface increases, therefore, the flow
rate may be safely increased as the evaporation
progresses to shorten evaporation time, if so desired.
Part No: AN857Issued year: 2016File size: 2.29mbFile type: pdf
This application note describes a protocol for the extraction of 1,25 di-OH Vitamin D2 and 1,25 di-OH Vitamin D3 metabolites from serum using supported liquid extraction prior to LC-MS/MS detection.
A calibration range between 5 and 500 pg/mL is demonstrated using a starting volume of 0.25 mL of serum. Sensitivity is maximized through the use of a simple PTAD derivatization and formation of a methylamine complex.
The method can be easily automated using the Biotage Extrahera. Details of the automated procedure and data comparing manual and automated method performance are included.
Part No: Issued year: 2011File size: 0.16mbFile type: pdf
Molecularly Imprinted Polymers (MIPs) are highly cross-linked polymers with selective binding sites engineered to contain recognition elements in defined positions1. MIPs have been developed for a large variety of small molecules, peptides, carbohydrates and even proteins. The schematic 0of a MIP site.
Part No: P055Issued year: 2013File size: 0.7mbFile type: pdf
Free urinary cortisol levels can be an indicator of a variety of disorders, such as Cushing Syndrome. This poster presents a simple method for the extraction of cortisol from urine demonstrating good recoveries and low ion suppression. LC-MS/MS analysis was performed using a Waters 2795 Liquid Handling Unit coupled to a Quattro Ultima Pt triple quadrupole MS using electrospray ionization, operated in the MRM mode. Supported liquid extraction method development resulted in recoveries greater than 90% for cortisol spiked urine. Calibration curves constructed using this method from 25-2000 ng/mL, demonstrated excellent linearity with coefficients of determination greater than 0.99.
Cortisol, Stress, Cushin's Syndrome, SLE, Supported Liquid Extraction, SPE, LLEMSACL, San Diego, 2013
Part No: Issued year: 2004File size: 0.39mbFile type: pdf
•Metal-mediated [2 + 3] cycloaddition to coordinated nitriles
-- synthesis of new transition metal complexes
-- synthesis of new heterocycles
-- enantioselective synthesis of heterocycles
role of microwaves?
• Platinum-catalysed cycloisomerisation of alkynes
-- Synthesis of Taxol-like compounds
-- highly efficient and atom economic chemistry
role of microwaves?
Part No: AN061Issued year: 2012File size: 0.63mbFile type: pdf
Acetone is successfully used as solvent in normal-phase flash chromatography when used with an Isolera™ Spektra flash purification system. The new λ-All detection and baseline correction features provide compound detection at all wavelengths in the detector’s range while minimizing any baseline drift due to solvent UV absorption.
Part No: PPS410Issued year: 2015File size: 0.7mbFile type: pdf
User Case: Professor Roger Strömberg, Karolinska Institutet. One of Professor Strömberg’s projects at Karolinska Institutet
involves the synthesis of artificial nucleases and PNAzymes. In
2013, his research group acquired a Biotage® Initiator+ Alstra™
peptide synthesizer for making PNAs and peptides.
Part No: PPS409Issued year: 2015File size: 1.61mbFile type: pdf
RIKEN is Japan’s largest research organization with 3,400
researchers from more than 50 countries. The chemists in RIKEN’s
Sugiyama Laboratory use EVOLUTE® EXPRESS solid-phase extraction
plates from Biotage in the analysis of clinical trial samples
for pharmacokinetic studies.
Part No: Issued year: 2013File size: 0.43mbFile type: pdf
User report: ISOLUTE SLE+. Shin Nippon Biomedical Laboratories, Ltd. use ISOLUTE® SLE+ to prepare biological samples for pharmacokinetic testing as part of a drug discovery and development program. We had the chance to speak with Mr. Mitsuhiko Kawabata and Ms. Akiko Toda of the pharmacokinetics group.
Part No: PPS406Issued year: 2015File size: 2.25mbFile type: pdf
Tokyo based PeptiDream Inc. is a company specializing in non-standard peptide therapeutics containing non-standard amino acids, and conducts research and development of new drug candidates. PeptiDream uses the peptide synthesizers Syro I and Biotage® Initiator+ Alstra™ for the synthesis of various kinds of peptides to support drug discovery and development.
Part No: AN042Issued year: 2003File size: 0.08mbFile type: pdf
Thin-layer chromatography (TLC) is a commonly used method development tool for flash purification. Product mixtures separated using TLC generally can be purified by flash chromatography using the identical solvent system. The method transfer accuracy of TLC to flash is based on the TLC silica and flash silica properties. When identical, the equation 1/Rf = CV holds, where Rf is the retention factor of a compound separated by TLC, and CV is the number of column volumes required to elute a compound. Cartridge loading capacity is based on the difference in CV (DCV) between two adjacent compounds.
Part No: Issued year: File size: 0.62mbFile type: pdf
The utilization of bound reagents for the solution phase synthesis has become an important tool in synthesis of biologically active molecules. The disadvantage of this technique is the relative slow rate of reaction. Microwave irradiation has been used to overcome this problem and increase rate of reaction of solid-assisted solution phase synthesis. This presentation covers developing efficient and robust strategies for the preparation of an array of cyclic tertiary amines using microwave irradiation in conjunction with bound reagents and scavengers such as MP-cyanoborohydride.
Part No: Issued year: 2015File size: 0.94mbFile type: pdf
The crossreactivity of molecularly imprinted polymers (MIPs) and its
practical implications are discussed. Screening of MIP libraries is presented as a
fasttrack route to discovery of resins selective towards new targets, exploiting the
fact that MIPs imprinted with one type of template molecule also show recognition
to related and sometimes also to apparently unrelated molecules. Several examples
from our own and others’ studies are presented that illustrate this crossreactivity and
the pattern of recognition is discussed for selected examples.