Part No: P023Issued year: 2008File size: 0.37mbFile type: pdf
Sample preparation is an essential technique prior to LC-MS/MS analysis of drugs in biological fluid samples to remove unwanted matrix components. These matrix components, particularly salts, proteins and phospholipids, can lead to ion suppression resulting in inaccurate quantitation and reduced detection limits. Resin-based mixed-mode cation exchange SPE sorbents are widely used for the extraction of basic compounds from biological fluids. The dual retention mechanism allows a two stage interference wash protocol, which results in extremely
clean extracts. This poster investigates the performance of EVOLUTE™ CX for overall ion suppression, then individual matrix components examined in terms of protein and phospholipid removal.
Part No: Issued year: 2005File size: 0.44mbFile type: pdf
PS-HOBt(HL) is a higher loading version (0.9 – 1.4 mmol/g) of a sulfonamide-linked,
resin-bound equivalent of 1-hydroxybenzotriazole (HOBt). PS-HOBt(HL) can be used as an effective activating reagent for transfer of protecting groups, e.g., Fmoc and Cbz, to amines.
Part No: Issued year: 2007File size: 0.26mbFile type: pdf
PS-TBD is a polymer-supported base, which
consists of a bicyclic guanidine moiety (1,5,7-
triazabicyclo[4.4.0]dec-5-ene) anchored on
polystyrene. PS-TBD is a stronger polymersupported
base than the PS-DIEA and PS-NMM
resins, which are bound tertiary amines that are
used in organic synthesis and reagent
scavenging. Published applications of PS-TBD
include alkylation of phenolsi and amines;ii
esterification of carboxylic acids using alkyl
halides; alkylation of activated methylene
compounds; de-halogenation of organic
halides;iii high throughput synthesis of aryl
triflates and aryl nonaflates,iv and the
regioselective synthesis of lysophospholipids.
Part No: Issued year: 2005File size: 1.52mbFile type: pdf
PS-DEAM is a polystyrene-bound diethanolamine, which is a resin-bound equivalent of the tridentate (N, O, O) N-alkyldiethanolamine ligand. PS-DEAM is an effective scavenger for a variety of oxophilic organometallic and inorganic complexes. The resin can be used to quench reactions and remove metallic reagents, catalysts or byproducts, allowing the purified product to be isolated by filtration. Boronic acids are scavenged by PS-DEAM. This has been exploited in the purification of Suzuki reactions through the removal of excess boronic acid and coupling byproducts.
Part No: Issued year: 2005File size: 0.38mbFile type: pdf
MP-Borohydride is a macroporous, polystyrene-bound borohydride, that is a resin-bound equivalent of tetraalkylammonium borohydride. The bound borohydride is a versatile reducing agent1,2,3 used for the reduction of carbonyl compounds and imines, and the reductive amination of aldehydes and ketones. The resin, in conjunction with some transition metal salts, can also be used for a number of other important reductive applications, such as reduction of oximes,
azides and alkyl halides. The reduced products are isolated by simple filtration away from the resin.
Part No: AN800Issued year: 2003File size: 0.05mbFile type: pdf
The automated Advantage Series™ 3400 ChemCorder™ workflow replicator was used to record all the manual operations a chemist performs during a highly exothermic chemical reaction (Figure 1).Before the experiment was initiated, the ChemCorder replicator was put in record mode.All steps of the experiment were accurately recorded, including any comments and observations. Once completed the ChemCorder replicator produced a report and recipe file of the chemistry. This recipe file was used to accurately and automatically repeat the reaction. Alternatively, the file could have been modified to produce a new recipe based on the recorded chemistry
Biotage® PRESSURE+ manifolds deliver positive pressure, parallel processing for 96 well plates,
1 mL 3 mL and 6 mL column formats. The systems utilize a consistent, uniform flow of positive pressure to move both low and high viscosity liquids through SPE plates and columns. Each port of the PRESSURE+ manifold independently maintains constant pressure, increasing the overall reproducibility of analyte recoveries. This unique design allows for partially populated racks to be used without sacrificing extraction efficiency.
Part No: Issued year: 2005File size: 0.3mbFile type: pdf
PS-DIEA is a high loading tertiary amine base which is a resin-bound equivalent of diisopropylethylamine. PSDIEA is useful in applications requiring a tertiary amine
base, where the resin-bound ammonium salt byproducts are readily separated by filtration.1 Synthesis of amides, sulfonamides and carbamates can be effected using filtration as the only purification step when PSDIEA is used in conjunction with PS-Trisamine or PSIsocyanate
as scavenger resins.
Part No: Issued year: 2005File size: 0.43mbFile type: pdf
PS-DMAP is a polymer-bound equivalent of dimethylaminopyridine (DMAP) which may be used as a catalyst for acylation and related reactions. PS-DMAP has a loading of 1.4 mmol/g based on nitrogen analysis. Typical catalysis conditions require 10 - 20 mol% relative to the nucleophile. Catalytic PS-DMAP accelerates the acylation of sluggish nucleophiles, e.g. tertiary alcohols.
Part No: Issued year: 2007File size: 0.09mbFile type: pdf
PS-TBD (Figure 1) is a polystyrene bound guanidine base, which is stronger than corresponding resin bound DIEA (DIPEA) and bound N-Methyl-morpholine resins. It has a wide variety of uses in synthesis, from direct alkylation through to sequestering of acidic components of reaction.
Part No: P005Issued year: File size: 1.34mbFile type: pdf
An oxidation method using a novel solid phase oxidant, based on a covalently polystyrene bound, sulfonic ester linked 2,2,6,6-tetramethylpiperidine-1-oxyl species is presented, PS-TEMPO (Fig.1a&1b).1,2 The reagent showed fast room temperature kinetics compared to similar known systems3 when used to oxidize primary and secondary alcohols to aldehydes and ketones, respectively (Table 1). The products were in general of high purity and the isolated yields were good to excellent. The used reagent could be reactivated and reused for multiple oxidation reactions. The colour change observed as the oxidation state of the reagent changed, gave an indication of the extent to which the reagent had been used.
Part No: TN521Issued year: 2003File size: 0.05mbFile type: pdf
PS-Thiophenol is based on an aminomethyl resin with a tethered thiophenol functionality. The resin was
designed for the scavenging of alkylating agents, e.g. alkyl halides. PS-Thiophenol was tested and found
effective in scavenging alkylating agents ranging from octyl bromide to benzyl bromide. The scavenging
effectiveness of PS-Thiophenol was found to be greater than a polymer-bound benzyl thiol towards octyl
bromide, indicative of the higher nucleophilicity of the thiophenolate.
Part No: TN513Issued year: 2003File size: 0.03mbFile type: pdf
PS-Trisamine is an amine functional resin for the removal of excess electrophilic reagents during the quenching and purification of reaction mixtures.1 PS-Trisamine resin has a scavenging capacity of 3.0–4.0 mmol/g based on reaction with an excess of benzoyl chloride. Scavenging of common electrophiles typically requires 3–6 equiv of PS-Trisamine and occurs within 0.5–3 h at room temperature. The scope of PS-Trisamine as a scavenger for electrophilic reagents was investigated using 4-chlorobenzoyl chloride, 2-phenylbutyryl chloride and 2,6-dimethoxybenzoyl chloride as a series of acid chlorides with decreasing
reactivity.Acid chlorides were completely scavenged in 0.5 h using 3.5 equiv PS-Trisamine (Table 1). The presence of a tertiary base, e.g. PS-DIEA or PS-NMM, reduces the amount of PS-Trisamine required in the reaction by removing the hydrogen chloride formed. In addition to acid chlorides, benzenesulfonyl chloride and 4-methoxyphenyl isocyanate were effectively scavenged in 0.5 h.
Part No: TN123.06Issued year: 2006File size: 0.07mbFile type: pdf
This Chemistry Data Sheet details the use of ISOLUTE PE-AX, a strong anion exchange sorbent, for the
purification of acidic products from organic synthesis mixtures containing non-acidic reagents or by-products.
Part No: Issued year: 2013File size: 0.67mbFile type: pdf
We have successfully developed a rapid and efficient microwave-assisted protocol for the preparation of Neu5Ac congeners that are important intermediates for clinically-relevant derivatives of Neu5Ac. The syntheses were performed using readily available reagents, improved on established techniques, and used more benign reagent for peracetylation. Moreover, the protocol that we developed is 1 to 2 orders of magnitude faster than conventional methods.
Initiator+ SPWave synthesis system
Dhananjaya Sahoo, I. Abrrey Monreal, and Jonel P. Saludes
Part No: Issued year: File size: 0.18mbFile type: pdf
For high efficiencyin parallel synthesisand method developement short reaction timesare essential. We have examinedthe possibilityof maintaining reported selectivitiesin rapid, high temperaturepalladium-catalyzed asymmetric allylic alkylations. Reactions were promotedby useof singlemode microwave heating(vide infra),which oppositeto conventional oilbath heating(wallheat transfer) rapidlyand almost homogeneouslyheat largeparts of the sample(internalheat transfer).
Part No: Issued year: 2011File size: 0.18mbFile type: pdf
User report: RapidTrace. The Laboratory of Racing Chemistry (LRC) analyzes samples from racehorses for doping drug. In order to screen approximately 1000 samples per week, LRC use an array of Biotage RapidTrace automated SPE systems. In an interview, Mr. Kenji Kinoshita and Mr. Kensaku Shirai talked about their experiences with the RapidTrace system in processing the heavy workload.
Part No: AN704Issued year: 2011File size: 0.04mbFile type: pdf
This Application Note describes the operating conditions for the automated fractionation of EPH into aliphatic and PAH fractions using the ISOLUTE EPH column in conjunction with the RapidTrace SPE automation system.
EPH, Massachusetts Department of Environmental Protection,
Part No: RT-BR-01Issued year: 2010File size: 0.84mbFile type: pdf
Advanced bioanalytical techniques like LC/MS/MS and GC/MS are meeting the increasing demand for greater speed and specificity in toxicological screening. But conventional sample preparation methods have not kept pace. In particular, solid phase extraction (SPE), an essential step in the analysis of many biomolecules, has become a through-put limiting step in many laboratories.
The RapidTrace+ is a robust automated platform for quickly developing rugged, reliable SPE methods in regulated
pharmaceutical, clinical and forensic laboratories. The RapidTrace+ eliminates SPE bottlenecks so you can realize the
full benefits of today’s powerful analytical instruments.
Part No: AN062Issued year: 2012File size: 1.44mbFile type: pdf
Pure fractions are in high demand – impurities mean more work after purification. With new technology, fraction purity can be digitally analyzed directly during chromatography to reveal any problems on the fly. In this application we will show how the Isolera Spektra is used to determine fraction purity, eliminating the need for other post-purification analysis.
Part No: Issued year: 2006File size: 0.68mbFile type: pdf
Synthetic oligosaccharides and glycoconjugates provide materials for correlating structure with function. Synthetic mimics of the complex assemblies found on cell surfaces can modulate cellular interactions and are under development as therapeutic agents.
Part No: P056Issued year: 2013File size: 0.42mbFile type: pdf
We detail here the application of new column technology to purify histamine and serotonin (Table 1) in one extraction method with the elimination of the sorbent conditioning and equilibration steps familiar to traditional solid phase extraction (SPE) method protocols prior to measurements by ultra performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-MS/MS). A secondary goal of combining two LC methods into one method was also achieved.
EVOLUTE EXPRESS cation exchange (CX), weak cation exchange (WCX) and acid-base-neutral (ABN) sorbents in a 96 well plate format prior to analysis by UPLC-MS/MS.
Part No: P014Issued year: 2006File size: 0.13mbFile type: pdf
One very common transformation in organic synthesis is the reduction of aldehydes or ketones to the corresponding primary or secondary alcohols (Scheme 1) using sodium borohydride as hydride donator. This reaction generally generates the product in very high yield. Among the draw-backs are long reaction times, that a large excess of reagent is needed and that the reaction mixture must be extracted in order to separate the inorganic salts from the product.
Part No: AN074Issued year: 2013File size: 0.52mbFile type: pdf
In this example, Isolera™ Dalton was used to fractionate completely non-UV absorbing starting materials and products from a classic reductive amination reaction. A resin bound cyanborohydride reagent was used to greatly facilitate the work flow by eliminating the need for traditional work-up, and the mixture applied to flash chromatography purification methods.