Part No: P158Issued year: 2017File size: 0.27mbFile type: pdf
As reversed-phase flash chromatography gains traction in
medicinal chemistry labs the need to monitor its cost and
safety are becoming more important. Commonly used
reversed-phase solvents typically include water with an
organic solvent such as methanol or acetonitrile – each
have advantages and disadvantages.
Part No: AN801Issued year: 2003File size: 0.27mbFile type: pdf
The heat flow parameter can be used to monitor the progress of a reaction, and can be useful
in determining reaction rates. A heat flow probe study was executed on the Advantage
Series™ 3400 process chemistry workstation for the hydrolysis of acetic anhydride in water
at temperatures from 25 to 55 °C. The observed rate constant for the hydrolysis was determined
from the heat flow measurements. An Eyring plot was produced and the enthalpy and
entropy of activation were determined. Finally, the heat of reaction was measured based on
the total amount of heat that was observed during the hydrolysis.
Part No: AN036Issued year: 2001File size: 0.55mbFile type: pdf
Activated carbon is an adsorbent media used to remove colored compounds from solution. Using this media in the Biotage FLASH-AC cartridge as a packed bed improves adsorbent performance. Increasing the temperature of the solvent modifies adsorption and alters performance of the decolorization process. Elevated temperatures increase product solubility, therefore requiring less solvent than at room temperature. The increased concentration of product in a hot solution also simplifies crystallization.
Part No: AN040Issued year: 2003File size: 0.4mbFile type: pdf
Research in CNS drugs is primarily centered on nitrogen heterocycle chemistry. Basic amines are difficult to purify using traditional silica chromatography because of strong interactions between acidic silica and the molecules’ basic amine groups. These interactions cause band spreading and poor compound recovery. Solutions employed to counteract this phenomena include adding a competing amine (e.g. triethyl amine or ammonium hydroxide) to the flash chromatography solvent system or using reversed-phase HPLC with a buffered solvent system.
Part No: P172Issued year: 2017File size: 0.49mbFile type: pdf
We investigate the use of reversed-phase high performance flash chromatography (HPFC) to quickly purify large quantities of crude synthetic peptides.
(6th Solid Phase Peptide Synthesis Symposium & 12th Australian Peptide Conference, Queensland, Australia, Oct. 2017)
Part No: Issued year: 2018File size: 0.66mbFile type: pdf
This poster presents a high sensitivity method for extraction and analysis of estrogens in human plasma. Sample preparation utilizes Biotage ISOLUTE SLE+ plates, providing high analyte recovery and low matrix effects.
MSACL 2018, Palm Spings, CA
Part No: AN041-HORIssued year: 2010File size: 0.83mbFile type: pdf
This application note investigates the applicability of automated solid phase extraction using the Biotage(r) Horizon 4790 extractor and DryDisk solvent drying system to extraction of a wide range of different compounds from phenols, to triazines, to organochlorine and organophosphorous pesticides spiked into tap water at a concentration of 1 ug/L.
Part No: Issued year: 2014File size: 0.34mbFile type: pdf
In this poster, an IONICS 3Q 220 triple quadrupole mass spectrometer using a load, wash, elute method protocol with recently advanced solid phase extraction (SPE) sorbent technology (EVOLUTE EXPRESS WCX) was used to perform analysis of the two compounds. As a result low levels of metanephrine and normetanephrine are detectable in plasma with short sample preparation and LC run times. This LC-MS/MS method provides a fast, sensitive, accurate, and reproducible solution for the analysis of ME and NME in plasma.
Part No: AN303Issued year: 2007File size: 0.14mbFile type: pdf
Heck reactions utilizing a thermostable catalyst in combination with microwave irradiation have been performed. A substantial enhancement of reaction rates as well as excellent regiocontrol could be obtained under microwave conditions without using inert gas. A slight increase in yield was also noted.
Part No: CM-HMPB-0810Issued year: 2010File size: 0.29mbFile type: pdf
For peptides acid, we recommend using the HMPB-ChemMatrix
as this resin will provide high crude purity and a recovery yield of
90-95%. The Wang-ChemMatrix will produce similar crude
peptide purity, but the recovery yield is lower (60-70%). On
request, we can provide preloaded HMPB-ChemMatrix resins with
all 20 naturally occurring amino acids. Other amino acids can be
preloaded on special request.
Part No: TN0171704_01Issued year: 2017File size: 1.18mbFile type: pdf
When a new piece of equipment is introduced the question is always raised about performance. Does it perform as well as its predecessor? What about the performance over time? This technical note will provide data to describe the performance of the SPE-DEX 5000, providing solid phase disk extraction (SPE), compared to standards required by environmental methods.
Part No: TN0101510_01Issued year: 2015File size: 0.45mbFile type: pdf
The quality of the solid phase disk used for extraction is key to the success and ease of an analysis. Horizon Technology’s Pacific™ Premium Oil & Grease SPE disks for Method 1664/ISO 11349 meet all Initial Precision and Recovery (IPR), Method Detection Limit (MDL) and Ongoing Precision and Recovery (OPR) limits specified by the US EPA, while saving the lab extraction time and solvent volume. Both 47 and 100-mm disks are fast-flowing and have a high-retention capability, which increases efficiency without compromising recoveries.
Part No: AN747Issued year: 2011File size: 0.18mbFile type: pdf
Biotage® PRESSURE+ manifolds deliver positive pressure, parallel processing for 96 well plates and 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. ISOLUTE SLE+ Supported Liquid Extraction plates and columns offer an efficient alternative to traditional liquid-liquid extraction (LLE) for bioanalytical sample preparation, providing high analyte recoveries, no emulsion formation and greatly matrix effects associated with biofluid analysis.
SLE+, SLE, Supported Liquid Extraction, positive pressure manifold, Pressure+96, Pressure+48
Part No: UI333Issued year: 2015File size: 0.89mbFile type: pdf
If high back pressure is detected in the makeup pump lines, and/or the High Makeup Flow Pressure dialog appears, the microfilter may be partially clogged and needs replacing. This is a step by step guide.
Part No: UI319.v3Issued year: 2017File size: 0.7mbFile type: pdf
Biotage®SNAP Ultra cartridges are compatible with CombiFlash® Rf Systems. As a convenience, Biotage SNAP Ultra cartridges with Luer slip connectors are available. Contact your Biotage representative for ordering information.
Part No: AN078Issued year: 2013File size: 1.05mbFile type: pdf
In this application note we demonstrate the power of mass detection in Isolera™ Dalton by investigating the incomplete separation of two dyes, Butter yellow (Mass 225.29 g/mol) and Sudan red (Mass 278.31 g/mol), by normal phase flash purification.
Part No: P053Issued year: 2013File size: 1.22mbFile type: pdf
Immunosuppressant drugs are extremely important for therapeutic drug monitoring (TDM) regimes, requiring robust and reliable methods for their analysis. This poster aims to demonstrate strategies for the extraction of various immunosuppressant drugs from whole blood providing clean samples prior to UPLC-MS/MS analysis. Spiked whole blood was extracted using a variety of protocols to investigate optimal combination of drug recovery and extract cleanliness. UPLC-MS/MS was conducted using a Waters ACQUITY UPLC coupled to a Quattro Premier XE triple quadrupole mass spectrometer. Acceptable extraction recoveries were obtained showing excellent extract cleanliness, demonstrating a reliable method for mass spectrometric approaches for these analytes.
Immunosuppressants, SLE, Supported Liquid Extraction, ISOLUTE, MSACL, San Diego, 2013
Part No: P140Issued year: 2016File size: 0.31mbFile type: pdf
Reversed-phase chromatography is typically used when you need to separate several milligrams of relatively polar compounds that either are not soluble in normal-phase solvents or are not compatible with bare silica
because they react, stick, or both. If you are currently using reversed-phase at preparative scale, such as flash chromatography, you know the mobile phase limitations – water with either methanol, acetonitrile, or
THF. As with normal-phase flash chromatography, when it comes time to purify you want your crude sample fully solubilized in the weakest possible solvent at the highest possible concentration.
Part No: AN044-HORIssued year: 2009File size: 0.65mbFile type: pdf
The Biotage® DryVap Concentrator System was intentionally designed to provide enhanced recoveries of semivolatile organic compounds (SVOC) such as those found in EPA Method 8270. The unique design of the DryVap system, which uses a vacuum, sparge gas, and internal immersion heater, allows it to achieve excellent recoveries for a wide range of compounds.
This purpose of this study is to determine the washing
technique for a DryVap® concentrator tube which
optimizes the recovery of both low and high boiling point
Part No: AN075.v2Issued year: 2013File size: 0.49mbFile type: pdf
In this application note we present a new type of polymeric reverse phase adsorbent that is able to provide improved separations of a range of small chemical compounds and also peptides evaluated side by side to a comparable benchmark DVB-Styrene macroporous resin.
MIP, molecularly imprint resins
Part No: AN063Issued year: 2012File size: 0.48mbFile type: pdf
Pyrazines are a class of organic molecules often used to provide flavor to foods. They are typically synthesized but some are found in fruits and vegetables, e.g. grapes, bell peppers, peas, asparagus, beetroot, tobacco, and roasted foods. Pyrazine’s heterocyclic chemistry can yield some challenges to their purification due to the various separation kinetics between the compound and silica. Biotage SNAP Ultra.
Part No: P160Issued year: 2017File size: 0.24mbFile type: pdf
Although capable of very high resolution, RP-HPLC is often limited by low column loading capacity, therefore demanding a significant time investment for peptide purification. As an alternative strategy, reversed-phase flash chromatography can also be used to purify synthetic peptides. The larger particle size used in flash column chromatography enables much larger loading capacity, thereby significantly reducing the time required for peptide purification.
Part No: PPS375.v1Issued year: 2015File size: 0.3mbFile type: pdf
User report: Flash instruments. Chugai Pharmaceutical uses Biotage flash chromatography products for drug discovery research. When deciding to convert from manual open-column procedures to automated systems, they chose successive generations of Biotage products, ranging from the Flash+® packed column to the Biotage® Horizon, SP1, Isolera™ Spektra, and Isolera™ Dalton automated flash chromatography systems.
Part No: AN041Issued year: 2001File size: 0.16mbFile type: pdf
Normal-phase flash purification is commonly used by organic chemists in pharmaceutical drug discovery and
process development labs. However, for many synthesized products (e.g. peptides, nucleotides and basic
drug candidates) purification on standard flash silica is not an option due to irreversible adsorption, chemical
interaction and/or solubility issues. Reversed-phase flash purification is an excellent solution for these applications. Yet, this technique has been used sparingly because of perceived lower loading capacity, higher
operating pressures and a scarcity of publications addressing reversed-phase flash chromatography.
Part No: AN082-HORIssued year: 2012File size: 0.85mbFile type: pdf
The focus of this Application Note is to illustrate some of the advances which have been made when performing EPA method 525.2 when using Solid Phase Extraction (SPE). It will make use of the Biotage(r) Horizon SmartPrep Automated Cartridge Extraction system set up to run in Bottle Rinse Mode with 6 mL SPE cartridges.
Part No: AN039Issued year: 2002File size: 0.64mbFile type: pdf
For pilot and production scale purification drugs, the use of a large particle-size media is common. Improving the purification throughput is limited by the media’s large particle size. Such a case was recently encountered when a pharmaceutical company attempted to improve the efficiency of a large-scale purification. In their current process, the use of a 350-600 µm polystyrene-type resin resulted in a lengthy purification cycle and low separation efficiency. However, the labile properties of the targeted component required a shorter purification cycle and high purification.
Part No: AN084-HORIssued year: 2012File size: 1mbFile type: pdf
Within EPA Method 549.2, the suggested rate to load a sample onto a solid phase cartridge is given as 3 to 6 mL/min.
This Application Note outlines the process used to extract diquat and paraquat from water samples using a faster loading rate than given by the EPA in method 549.2
Part No: TN128Issued year: 2006File size: 0.09mbFile type: pdf
This technical note describes the use of derivatization techniques to separate aliphatic
secondary amines from aliphatic tertiary amines in a mixture using the strong cation
exchange sorbent, ISOLUTE® SCX-2.
Part No: PPS385Issued year: 2015File size: 4.87mbFile type: pdf
Our carefully selected portfolio of industrial scale products have a proven track record of successful applications and use in scale-up projects. We can support the discovery, development and manufacturing of customer pharmaceutical and biotechnology products, from pre-clinical, phase I, II and III to small scale commercial operations.
Part No: TN-0028.1222Issued year: 2012File size: 1.6mbFile type: pdf
The Initiator+ is a flexible system that utilizes all Biotage vials, from 0.2 to 20 mL,
in any order or combination, at any time without system modifications, delivering greater flexibility and direct scale-up from milligrams to grams.
Part No: TN-0029.0611Issued year: 2011File size: 1.07mbFile type: pdf
In peptide synthesis mode, this is the perfect tool for chemists synthesizing peptides and peptidomimetics, including difficult modifications and labeling of sequences, by using single or multi-step procedures. The intuitive Initiator 4.0 software controls the instrument functions and by using the pre-defined methods, synthesis can be started immediately.
Part No: AN090Issued year: 2014File size: 1.95mbFile type: pdf
In mass detection, the presence of ions can suppress peaks
from the analytes of interest. This study concludes that
Isolera™ Dalton performs successful separations even with
ions present in the sample.
Part No: P181Issued year: 2018File size: 0.19mbFile type: pdf
Peptide purification using standard reversed phase HPLC methods are hampered by low loading capacity, resulting in purifications that demand significant time investment. Recently, the use of reversed phase flash chromatography has increased in popularity for peptide purification due to the significant reduction of purification time,
enabled by the increased loading levels of the larger stationary phase particles. Resolution, though, is somewhat diminished with the larger particle size, demanding creative techniques to retain a highly pure peptide product.
Part No: P180Issued year: 2018File size: 0.35mbFile type: pdf
In medicinal chemistry, organic synthesis will generate by-products with similar chemistry to the product. Separating these impurities from the product often becomes a challenge that often only prep HPLC can achieve.
In this poster, we discuss how using sample dry loading with a cation exchange scavenger media with flash chromatography
improves product purity by removing many of the impurities.
Part No: AN088.v1Issued year: 2014File size: 1.59mbFile type: pdf
Fragrance compounds, being invisible to UV, can be
elusive and difficult to isolate. In this application, a four
component mixture of fragrance compounds was purified
using Accelerated Chromatographic Isolation™ (ACI) and
identified by mass detection.
Part No: AN600Issued year: 2005File size: 0.08mbFile type: pdf
This Application Note reviews the use of ISOLUTE PPT+ plates for the isolation of drugs from biological fluids, including the method, recovery data and the impact of the filtrate’s cleanliness on analyte quantitation.