Part No: Issued year: 2003File size: 0.06mbFile type: pdf
Condensation reactions between N,N-dimethylformamide
diethyl acetal, DMFDEA, and compounds
comprising an activated methyl or methylene group
adjacent to a keto functionality form alkylaminopropenones.
These compounds have been used as
versatile intermediates for the synthesis of a large
number of heterocycles both with conventional and
Part No: P110Issued year: 2014File size: 0.25mbFile type: pdf
Corrosion costs the petroleum industry an estimated $1.3 billion in non-productive time, materials and labor annually. Imidazolines prepared from fatty acids and amines are a widely-used class of chemical corrosion inhibitor, due to excellent performance and ease of handling. However, commercial imidazolines are actually mixtures of several different chemical compounds, and the relative proportions of these species can have a large impact on both corrosion inhibition and product physical properties. The absence of gold standard analytical methods to characterize the active ingredients in imidazoline formulations limits the understanding of the chemistry of these materials. It is for this reason that a SPE-LC-MS method was developed to supplement the chemical information afforded by bulk testing / wet chemistry methods. It is anticipated that this method will have significant impact in the formulation of new corrosion inhibitors for oilfield applications as well as the quality control of finished products in manufacturing.
Part No: AN003-HORIssued year: File size: 0.16mbFile type: pdf
This study shows that the SPE-DEX® 4790 Automated Extractor system can process water samples containing suspended particulate matter, up to 1000 mg, for the analysis of PAH’s. As PAH’s are found in both the dissolved and particulate phase of the water sample, it is important to be able to handle “whole” water samples such that the particulate matter in the water sample is retained and extracted with the SPE disk. This filtration method ensures that the PAH’s found in the dissolved phase, and those adsorbed onto the particulate matter are properly
Part No: P116Issued year: 2014File size: 0.45mbFile type: pdf
This poster details current sample preparation strategies for aminoglycoside antibiotics in meat developed in a collaborative effort with Biotage and Tyson Foods, Inc. Springdale Corporate Laboratory to optimize analyte recovery (>70%), minimize analyte suppression and maintain acceptable method precision.
FAST LC-MS 2014
Part No: P070Issued year: 2014File size: 0.55mbFile type: pdf
This poster describes a strong cation exchange SPE protocol for extraction of Vitamin B3 (Niacin) and related metabolites from serum.
The ISOLUTE SCX-3 96 well plate format demonstrated as a viable option for serum measurements over a relevant concentration range in clinical diagnostics.
It is anticipated that strategies presented in this poster would be of broad-based interest to clinical laboratories focused on combining parent/metabolite assays into a single analysis.
Part No: AN814Issued year: 2014File size: 1.19mbFile type: pdf
This application note describes the extraction of Vitamin B3 (Niacin, nicotinic acid) and its key metabolites from serum using a strong cation exchange SPE retention mechanism. High reproducible analyte recoveries are achieved.
Part No: P052Issued year: 2013File size: 0.48mbFile type: pdf
Pain management therapy warrants constant monitoring of therapeutic levels of prescribed drug levels in patient urine samples. The number of samples being submitted for analysis has increased dramatically in the last 10 years with improvements in high throughput automated screening capabilities. Patient samples analysis is complicated by the need for an effective sample preparation methodology that can extract target analytes from complex matrices with good efficiency. Further complicating the process is the need to enzymatically hydrolyse the glucoronidated metabolites prior to extraction from the urine matrix. A fully automated sample preparation process using a TECAN Freedom EVO® 100 was designed to incorporate both the enzymatic hydrolysis and subsequent sample preparation assay as one continuous workflow. Supported Liquid Extraction (ISOLUTE SLE+) which offers an efficient alternative to traditional liquid-liquid extraction (LLE) and solid phase extraction (SPE) techniques was used to extract a suite of pain management drugs from spiked urine samples. A recovery and quantitation assay was run on the TECAN Freedom EVO® 100 using mock patient samples to demonstrate utility of automation process.
MSACL, Pain Management, Biotage, SPE, SLE, LLE, Supported Liquid Extraction, Drugs, MSACL, San Diego, 2013
Part No: Issued year: 2014File size: 0.88mbFile type: pdf
This poster presents the synthesis of peptidoglycan fragments where the coupling of peptides and carbohydrates was achieved using microwave heating. The fully automated total synthesis of a complex branched peptide is also presented. The fragments were synthesized using Biotage® Initiator+ SP Wave, Biotage® Syro Wave™ and Biotage® Initiator+ Alstra™ respectively. Presented at EPS, Sofia, 2014.
Part No: P047Issued year: 2012File size: 0.6mbFile type: pdf
The potential harm caused by synthetic cannabinoids is a significant concern since exposures and reports of human fatalities due to these substances is widespread . Detection of these relatively new type designer drugs in blood is essential in forensic toxicology, other scientific and medical fields.
Cannabinoids, SLE, SLE+, Supported Liquid Extraction,
Part No: AN818.v1Issued year: 2014File size: 1.54mbFile type: pdf
This application note describes the extraction of ethyl glucuronide and ethyl sulfate from human urine using ISOLUTE® NH2 solid phase extraction columns. The method has been applied real patient samples that had been previously analyzed with a validated referee method. The results of the orthogonal measurements agreed, to provide similar diagnostic values.
Part No: P144Issued year: 2016File size: 0.6mbFile type: pdf
The ability to extract a broad range of different drugs from a biological matrix allows for the expedited analysis of a patient sample using LC-MS/MS. Typically small molecules are extracted from matrices like urine based on their polarities. A fast and reliable sample preparation method that could be implemented to extract drugs of different polarities from urine could be used as a screening tool to quickly identify the presence of illicit drugs in patient samples using LC-MS-MS.
This poster demonstrates the utility of supported liquid extraction for the extraction of over 30 different acidic, basic and neutral drugs in urine prior to LC-MS/MS.
Part No: P035Issued year: 2012File size: 0.26mbFile type: pdf
Vitamin D deficiency can result in various health issues such as osteoporosis, liver and kidney problems and is associated with increased risk of cancers and multiple
sclerosis. From this standpoint vitamin D analysis has extremely important clinical relevance. This poster presents a novel method for the extraction of 25 hydroxyvitamin D demonstrating acceptable validation parameters from serum calibrators and DEQAS supplied samples using ISOLUTE SLE+.
Part No: P109Issued year: 2014File size: 0.43mbFile type: pdf
This poster describes a supported liquid extraction method for extraction of a class of novel psychoactive substances (NBOMes) with analysis using laser diode thermal desorption (LDTD) MS/MS. Samples are oral fluid collected using Salivettes.
Part No: P081Issued year: 2014File size: 0.42mbFile type: pdf
This poster describes a reduced workflow solid phase extraction method for extraction of vitamin B7 (biotin) from human serum. Using EVOLUTE EXPRESS AX 96-well plates, the traditional sorbent conditioning and equilibration steps are not required, meaning the sample can be applied directly to the dry plate. Post extraction evaporation is also eliminated.
Part No: P091Issued year: 2014File size: 0.38mbFile type: pdf
This report details a “load, wash, elute” weak cation exchange solid phase extraction procedure amenable to both plasma and urine samples. The extracts are subsequently injected into an LC-MS/MS system. The preliminary sample preparation method was developed at the Biotage US Applications lab (Charlotte, NC).The method was then transferred to Ionics (Bolton, ON, Canada) to facilitate the nmole/L measurements of the selected biomarkers
by laminar flow tandem mass spectrometry. The SPE-LC-ESIMS/ MS method parameters were first optimized using pooled mixed gender plasma. A set of patient samples (n=32) was later supplied by the Mayo Clinic (Rochester, MN) that had previously been analyzed by a validated referee method. The population represented measured values across a range of clinical relevance.
Part No: P183Issued year: 2018File size: 1.3mbFile type: pdf
The compound 4 Methylimidazole (4-MeI) is made during the production of caramel color commonly found in foods and beverages, especially sodas.
The Codex Alimentarius of the World Health Organization sets a limit of 250 mg/kg of 4-MeI. Also, the state of California has added 4-MeI to its Prop 65 list at an exposure level of 29 μg/day.
This study looks at 4-MeI levels in sodas and malt sodas which
are sold in and outside the state of California. The first section, included in this poster, describes the performance of automated solid
phase extraction of 4-MeI using conventional HPLC/MS detection.
ASMS 2018, San Diego, CA
Part No: P044Issued year: 2012File size: 0.89mbFile type: pdf
The objective was to develop a GC-MS assay for the determination of free benzodiazepines using Supported Liquid Extraction (SLE). The SLE extraction mechanism is very efficient, delivering higher analyte recoveries and cleaner extracts than equivalent LLE methods.
ISOLUTE, SLE, SLE+, Supported Liquid Extraction, Benzodiazepines, Forensic, Drugs, DOA, Drugs of Abuse, SOFT,
Part No: Issued year: 2016File size: 0.94mbFile type: pdf
Cortisol measurement in hair samples scan be a useful indicator of chronic stress. This poster compares a new LC-MS/MS method with an existing immunoassay based method.
The Biotage Bead Ruptor is used effectively for hair pre-treatment.
Part No: P159Issued year: 2017File size: 0.25mbFile type: pdf
When it comes to polar organic compound purification,
many chemists turn to normal-phase flash
chromatography often utilizing dichloromethane and
methanol as the eluting solvents. While this can work, it
often can be challenging to optimize due to methanol’s
high polarity and protic chemistry.
Part No: MSACL US 2018 Breakfast SeminarIssued year: 2018File size: 3.24mbFile type: pdf
The use of LC/MS analysis in the clinical lab has increased exponentially over the last 10 years. Modern mass spectrometers are extremely sensitive allowing low level detection of many target analytes. However, this sensitivity can come at a price, in that levels of contamination not previously detected with less sensitive instruments can now have larger impact on analysis. The complexity of common matrices such as plasma/serum and urine while presenting different challenges can have a marked influence on method performance.
As a result sample preparation is an extremely important part of the process in order to provide robust methods. This seminar focuses on some of the method development challenges our lab faced when looking at two clinical assays:
Endogenous steroid hormone extraction from serum, and catecholamine extraction from plasma and urine.
Particular emphasis is placed on the various sample preparation options we looked at for the extraction of these analytes. During optimization of the extraction process we investigated analyte recovery, co-extractable matrix components, HPLC column degradation, calibration curve performance and limits of quantitation.
MSACL US 2018 Breakfast Seminar
Part No: TN-0022.0207Issued year: 2007File size: 0.08mbFile type: pdf
ACTU Preparation of PS-HOBt(HL). 2-Chloro-1,1,3,3 tetramethyluronium hexachloroantimonate (ACTU) is a reagent which allows polymer-supported active esters of PS-HOBt(HL) to be prepared in pure DMF. ACTU addresses the problem that many carboxylic acids are not soluble in DCM.
Part No: PPS457Issued year: 2017File size: 0.02mbFile type: xlsx
Use this simple tool to look up possible adducts and fragments which may occur with Isolera™ Dalton or Biotage® Dalton 2000 mass detectors.
Enter the target compound weight and use the mass lookup cell to highlight resulting m/z values.
Part No: Issued year: 2008File size: 0.2mbFile type: pdf
Advancer Kilobatch provides up to 12 hours unattended processing of homogenous reaction mixtures delivering kilogram quantities of your target compound. In addition, the system
will accommodate heterogeneous reactions by processing four sequential cycles (250 mL) to yield a 1 L batch. Through simple solid loading replenishment, kilogram quantities of
complex heterogeneous reactions are easily achieved.