This study shows the use of the GERSTEL MPS 2/TDU/CIS with pyrolysis module for generating simulated thermal gravimetric-mass spectrometry data (TGA-MS) of polymer samples. This mode of operation is also referred to as evolved gas analysis (EGA). For EGA analysis, a short piece of uncoated capillary is attached from the GC inlet to the mass…
The US Consumer Product Safety Commission’s (CPSC) Test Method CPSC-CH-C1001-09.3 [1], is used by testing laboratories for the determination of phthalate content in children’s toys and child care articles covered by the standard set forth in the Consumer Product Safety Improvement Act Section 108. The CPSC determined that an appropriate combination of methods of extraction…
This note presents the automated determination of benzo[a]pyrene and benz[a]anthracene in tar distillation products by SPE-GC/MS. Samples are dissolved in tetrahydrofuran (THF), placed in sample vials and internal standard added. The vials are then placed in the autosampler. All further sample preparation steps which include SPE cleanup on silica gel cartridges and injection into the…
The analysis of airborne aldehydes and ketones first involves collection of the analytes by passing air through a cartridge containing 2,4-dinitrophenylhydrazine (DNPH). As the air passes through the cartridge, the analytes react with the DNPH to form hydrazones which are immobilized on the cartridge. The cartridges are then eluted with solvent and the DNPH derivatives…
Forensic laboratories face the need to analyze many samples of human blood and body fl uids for alcohol content. The large number of samples that require quantification of ethanol in these facilities creates a challenge for the methodology employed. Factors that need to be considered are sample throughput, resolution, and carryover. A successful method for…
Proposed revisions to the DHHS Mandatory Guidelines for Federal Workplace Drug Testing Programs [1] (Federal Register, April 13, 2004) include a confi rmatory cutoff level of 2.0 ng/mL for THC (parent) in oral fl uid. The relatively low cutoff level and small specimen volume (versus the corresponding parameters for urine drug testing) present a challenge…
An experimental biocompatible stir bar sorptive extraction (SBSE) device was prepared using a restricted access material (RAM) as the SBSE coating. The biocompatible SBSE approach was advantageous in terms of simplifying the sample preparation procedure. The RAM-SBSE bar was able to simultaneously fractionate the protein component from a biological sample, while directly extracting caffeine and…
Stir bar sorptive extraction (SBSE) is an innovative sample extraction technique that can be used to process blood, urine, and tissue samples for routine drug screening in the forensic toxicology laboratory. The GERSTEL TDU System is a multifunctional thermal desorption unit capable of determining the presence of analytes from liquid samples after extraction using the…
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…