Solid phase microextraction (SPME) is a powerful technique for the analysis of trace components in a wide variety of matrices. The types of compounds which can be analyzed by this technique ranges from non-polar to semi-polar materials due to the different fiber materials available. Most applications favor headspace over immersion sampling, therefore the analytes must…
Reduction in analysis time is an important goal for easing the burden of large sample sets associated with routine screening of blood samples and sample sets produced from drug metabolism studies. This study focuses on reduction in analysis time for simultaneous detection of delta-9-THC, 11-OH-THC, and THC-COOH in whole blood and urine extracts. This was…
Disposable Pipette Extraction (DPX) has been shown to be a rapid, efficient and reproducible technique for performing solid-phase extraction (SPE) of drugs from biological specimens. DPX is based on pipette tips that incorporate loosely contained sorbent material. The sorbent is suspended in the sample solution using turbulent air bubble mixing for efficient contact between the…
In this work an automated DPX procedure is presented that enables the determination of acidic, basic, and neutral drugs in small blood or urine samples. The DPX method is based on a mixed-mode cation exchange sorbent (CX) with reversed phase characteristics. The automated extraction is shown to require only minimal manual labor when performed using…
Solid phase extraction (SPE) is one of the sample preparation methods most widely used by chromatographers, as demonstrated by the numerous published 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 adsorbent can…
The analysis of opiates in blood and urine was accomplished using automated Disposable Pipette Extraction (DPX) followed by LC/MS analysis. The automated extractions were performed in about 5 minutes using a GERSTEL MultiPurpose Sampler (MPS). The eluents were subsequently dried and reconstituted in solvent and injected into a HPLC/MS/MS instrument. Recoveries ranged from 60 to…
Solid phase extraction (SPE) is a widely used, proven method for sample preparation and sample clean-up in the field of forensic analysis. A number of SPE products are available that offer various sample preparation functions and cover a wide range of procedures. Most SPE products require relatively large volumes of solvent leading to increased time…
Stir Bar Sorptive Extraction (SBSE) is an innovative and efficient method [1] for the extraction of drugs and pharmaceuticals from blood-, urine- and tissue samples in a forensic toxicology laboratory. As shown in this application note and earlier publications [2,3,4], SBSE is an effective screening tool for drugs and pharmaceuticals in biological fluids and tissue.…
Solid phase extraction (SPE) is a widely used, proven method for sample preparation and sample clean-up in the field of forensic analysis. Most SPE products, however, are designed in such a way that relatively large volumes of solvent are required for the process. Consequencently, sample processing times, cost per sample, as well as limits of…
This study focuses on the automated extraction of small volumes of urine samples (< 500 μL) using disposable pipette extraction (DPX) for the comprehensive screening for pain management drugs by LC-MS/MS. Using a GERSTEL MPS autosampler, DPX extractions of hydrolyzed urine were performed, using a reversed phase (DPX-RP-S) sorbent. The resulting eluents from the DPX…
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…