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 microwave heating.
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. GCC 2014
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 extracted.
Acenaphthene Acenapthalene Anthracene Application Notes Benzo(a)anthracene Benzo(a)pyrene Benzo(b)fluoranthene Benzo(ghi)perylene Benzo(k)Fluoranthene Chrysene Dibenzo(ah)anthracene Disk English Environmental Fluoranthene Fluorene GC-MS Indeno(123-cd)pyrene PAHs Persistant organic pollutants (POP) Phenanthrene Polyaromatic Hydrocarbons (PAH) Pyrene
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
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. MSACL 2014
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.
This application note describes the extraction of nine phthalate metabolites from human urine using ISOLUTE® ENV+ solid phase extraction columns.
Application Notes Biomarker Clinical Column English LC-MS/MS Mono(2-ethyl-5-carboxypentyl) phthalate (MECPP) Mono(2-ethyl-5-hydroxyhexyl) phthalate (MEHHP) Mono(2-ethylhexyl) phthalate (MEHP) Monobenzyl phthalate (MBzP) Monobutyl phthalate (MBP) Monoethyl phthalate (MEP) Monohexyl phthalate (MHxP) Monoisononyl phthalate (MiNP) Monomethyl phthalate (MMP) Phthalate Metabolites Phthalates Urine
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
6-acetylmorphine (MAM) 96-well plate Benzodiazepines Clinical Clonazepam Codeine Diazepam Dihydrocodeine (DHC) Drugs of Abuse Flunitrazepam Hydrocodone Hydrolysed urine Hydromorphone LC-MS/MS Methadone Methamphetamine Morphine Nitrazepam Opiates Oxycodone Oxymorphone Posters Urine
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.
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,
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.
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. MSACL 2016
11-hydroxy- Δ9-tetrahydrocannabinol (THC-OH) 11-nor- Δ9-carboxy tetrahydrocannabinol (THC-COOH) 6-acetyl codeine 96-well plate Acidic Alprazolam Amphetamine Barbiturates Basic Benzodiazepines Benzoylecgonine Buprenorphine Butalbital Clinical Clonazepam Codeine Dextromethorphan Diazepam Drugs of Abuse EDDP English Fentanyl Flunitrazepam Forensic Hydrocodone Hydrolysed urine Hydromorphone LC-MS/MS MDEA Morphine Naltrexone Neutral Nitrazepam Norbuprenorphine Norcodeine Norfentanyl Opiates Oxazepam Oxycodone Oxymorphone Pain Management Pentazocine Pentobarbital Phenobarbital Posters Propoxyphene Secobarbital THC THC metabolites THC-COOH Temazepam Δ9-tetrahydrocannabinol (THC)
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+.
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. TAMS 2014
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. ASMS 2014
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. AACC 2014
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