This study focuses on the rapid cleanup of urine samples (< 500 μL) using disposable pipette extraction (DPX) for high throughput LC/MS/MS screening of buprenorphine (Bup) and main active metabolite norbuprenorphine (Nbup). Using a GERSTEL MultiPurpose Sampler (MPS), DPX extractions of hydrolyzed urine were performed, and analysis results were directly compared to results obtained using…
This application note describes a fully automated analysis method for selected equine doping compounds in equine urine. A GERSTEL MultiPurpose Sampler (MPS) with Disposable Pipette Extraction (DPX) option is employed for extraction and cleanup. After gas chromatographic separation the analytes are detected by a triple-quadrupole mass spectrometer (QqQ-MS). The method is rugged, provides an adequate…
This work demonstrates the use of disposable pipette extraction (DPX) as a fast and automated sample preparation technique for the determination of barbiturates and 11-nor-9-carboxy- 9-THC (COOH-THC) in urine. Using a GERSTEL MultiPurpose Sampler (MPS) with DPX option coupled to an Agilent 6460 LC-MS/MS instrument, 8 barbiturates and COOH-THC were extracted and their concentrations determined.…
This application demonstrates the use of Disposable Pipette Extraction (DPX) for rapid, automated sample preparation of urine samples for comprehensive LC/MS/MS screening. The combination of automated sample cleanup and introduction with mass spectrometric detection using a Scheduled MRM™ (AB SCIEX) algorithm and fast MS/MS spectral acquisition allowed high confi dence compound identifi cation based on…
Analyzing blood serum for opioids, cocaine and metabolites is a routine task in forensic laboratories. The most commonly used methods involve several manual or partly-automated sample preparation steps such as protein precipitation, solid phase extraction, evaporation and derivatization followed by GC/MS or LC/MS determination. In this study a comprehensively automated method is compared with a…
A major mechanism of the metabolism of many pain management drugs involves conjugation of the analyte with glucuronic acid. To ensure accurate results when drugs are determined from urine matrices the analytes must be deconjugated which is typically performed by hydrolysis using enzymes such as beta-glucuronidase. Typical hydrolysis procedures involve long incubation periods at specified…
This note presents a fully automated analysis system for the determination of Δ9-tetrahydrocannabinol (THC) and its metabolites in blood serum. Automation is based on the GERSTEL MultiPurpose Sampler (MPS) equipped for solid phase extraction (GERSTEL SPE) and a module for automated eluate evaporation (GERSTEL MultiPosition Evaporation Station, mVAP). A validated, semi-automated analysis method used for…
In this report, a completely automated, 96 well plate format “Prep-and-Shoot” workfl ow including enzymatic hydrolysis, dilution and injection is described. A GERSTEL MultiPurpose Sampler (MPS) coupled to an AB SCIEX QTRAP® 4500 LC/MS/MS system was used for a fast enzymatic hydrolysis process (15 minutes), dilution and injection of urine samples. The procedure was applied…
Liquid-liquid extractions have long been performed manually and are used to extract and concentrate analytes from aqueous matrices. Inclusion of liquid-liquid extraction in many official methods attests to the wide acceptance of the technique. Following solvent extraction it is also common to include an evaporation and reconstitution step to improve detection limits or exchange solvents…
The extraction of dried blood spots (DBS) typically involves manual intervention. First, a small disc is punched out of the center of a dried blood spot placed on a DBS card. Following solvent extraction of the sample, it is also common to include further cleanup steps, using solid phase extraction (SPE) to improve detection limits…
Solid phase extraction (SPE) is one of the sample preparation methods most widely used by chromatographers, as can be seen from the large number of SPE methods found in the literature. Typically, a liquid sample is passed across an adsorbent bed to retain and concentrate target analytes and eliminate interference from the sample matrix. Alternatively,…
The Opioid Epidemic continues to increase throughout the United States. According to the CDC, 66 % of all drug overdose deaths in 2016 involved an opioid [1]. This calculates to roughly 116 deaths every day from opioid related overdoses. After becoming addicted to prescription opioids, users may unfortunately turn to illicit alternatives such as heroin.…
Packaging materials for foodstuffs or consumer usage must not alter the fl avor or odor of the substance being packaged. Examples of packaging materials include the paper used to wrap cigarettes, the paper cartons used in orange juice or milk and the Polyethylene (PE) often used for caps to seal soft drink bottles. Sometimes, due…
Analysts often encounter complex real-world sample types such as petroleum fractions or volatile polymer components. Resolving all individual compounds using a single chromatographic separation can be quite challenging. Coupling columns with different polarities (multidimensional GC) can signifi cantly improve the resolution of complex samples. We coupled two low thermal mass (LTM) GC column modules with…
The quality of packaging materials used in the food and beverage industry must be controlled regularly in order to avoid negative effects on packaged products caused by emissions, e.g. VOC emissions from printing processes or from varnishes used on inner surfaces of the packaging material. Many companies have worldwide production sites, that may not all…
Direct thermal extraction is a sensitive technique for the analysis of residual compounds in solid matrices such as polymers, films, powders, and fibers. This approach can be used for both qualitative identification of unknowns as well as quantification of trace components. Quantification of analytes is often performed based on off-line spiking of liquid or gaseous…
This paper describes an automated pyrolysis system for gas chromatography (GC) based on a filament type pyrolyzer combined with a commercially available thermal desorption instrument, onto which the pyrolysis module is installed. Automated sample introduction for both pyrolysis and thermal desorption is performed using a commercially available autosampler. For pyrolysis of solid, liquid, or melting…
This application note describes two automated methods for screening of extractable compounds from materials for food packaging, medical or technical purposes. The first method is based on automated liquid extraction performed by the GERSTEL MultiPurpose Sampler (MPS), the second involves thermal desorption of the material in question in the GERSTEL Thermal Desorption Unit (TDU). Both…