01/12/20171.EtG/EtS Analysis in Urine
Ethyl glucuronide (EtG) and ethyl sulfate (EtS) are conjugated ethanol biomarkers. Due to their highly polar nature (log P of 1.51 and 0.62, respectively) and lack of retention on a traditional reversed phase HPLC column, their analysis is typically plagued by significant ion suppression when using a standard Dilute & Shoot approach. By utilizing UCT’s Clean Screen® FASt EtG filter and shoot columns in conjunction with the Selectra® EtG HPLC column, a quick and efficient overall clean-up and analysis can be executed allowing for purified extracts, significant improvements in LOD/LOQ’s, in addition to enhanced analytical column lifetime.
2. The Analysis of Δ9-THC and Its Main Metabolites in Whole Blood
While these compounds have been major players in a toxicological setting for quite some time, there still appears to be a generalized struggle to precipitate and extract them efficiently from whole blood. Not only is the ratio of acetonitrile to blood sample critical for proper precipitation of these highly protein-bound compounds, but also the speed in which it’s added along with the working temperature of the solvent at hand. Typically, for a 1 mL blood sample, 2-2.5mL of ice-cold acetonitrile should be added in a dropwise fashion while simultaneously vortexing. Following centrifugation, the supernatant should then be cleaned-up on a solid-phase extraction media such as UCT’s StyreScreen® THC column prior to instrumental analysis
3. Baseline LC Separation of Isobaric Compounds
The ability to separate complex mixtures of structurally similar compounds within one method is highly desirable. Additionally, compounds of related structures may also be isobaric with similar fragmentation, rendering them unidentifiable by MS/MS. In these cases, it is essential that these compounds be baseline separated chromatographically. Several compound duos that require baseline separation for accurate quantitation have been successfully resolved using UCT’s Selectra® DA HPLC column including 2C-phenethylamine isomers, Ephedrine and Psuedoephedrine, Methamphetamine and Phentermine, and Ethylone and Butylone. By choosing the correct column chemistry, mobile phase combination and gradient, baseline separation can be accomplished when needed.
4. Enzyme Hydrolysis Rates for Opiates
The hydrolysis of morphine-3-glucuronide and various other conjugated drug classes such as benzodiazepines and synthetic cannabinoids is routinely fast and efficient. Other compounds prove to be more difficult to covert, such as codeine-6-glucuronide, due to the nature of the chemical bonds at hand and the configuration of the enzyme to the substrate. Derived from red abalone, UCT’s Abalonase™ requires as little as 5,000 activity units per milliliter of sample in order to achieve conversion rates of over 80% for both morphine-6-glucuronide and codeine-6-glucuronide. This purified and clear enzyme reduces average hydrolysis time when compared to traditional formulations while keeping cost per sample down thanks to less activity units needed when comparing to other purified products in the market.
5. Opiate Derivatization
Multiple strategies can be used to derivatize opiates prior to analysis on GC-MS. A variety of both silylation and acylation reagents can be used to best accomplish this, including either BSTFA (with 1% TMCS) or Propionic Anhydride (PIA). When using BSTFA, a hydroxylamine solution can be added to the sample following hydrolysis if the oxime derivative is desired. This additional step allows for single derivatives of hydromophone and hydrocodone to be observed, in addition to increased retention times. This provides better separation from morphine and codeine, respectively. Both ultra-pure BSTFA and PIA are available in UCT’s line of Selectra-Sil® derivatization reagents.
6. Cannabis Analysis
Even within states where recreational cannabis has not been legalized, government funded crime laboratories are seeing an uptick in seized plant and edible cannabis cases. While toxicology sections are equipped with the tools needed to extract said samples if tasked with this additional work, drug chemistry units may struggle to treat the various edible forms, tinctures and waxes that appear in their laboratory. Using the QuEChERS (Quick, Easy, Cheap, Rugged and Safe) extraction approach provides a fast and efficient way to clean up numerous types of cannabis matrices without sacrificing your instrument and column in the process. Perfect for qualitative analysis, UCT’s QuEChERS salt blends can be customized to fit your laboratory’s needs, without requiring any extensive training for your technicians.
7. Identification and Extraction of Fentanyl and Its Newly Emerging Analogues
It goes without saying that fentanyl related overdoses and deaths were a major public health issue across the United States in 2016 and will continue to be in the upcoming year. Forensic toxicologists need fast and accurate extraction methodologies in order to not only identify fentanyl but also additional novel analgesics that may be isolated in casework screening protocols. UCT’s Clean-Screen® XCEL I solid phase extraction columns allow for the elimination of conditioning steps and the reduction of wash steps, leading to a faster overall extraction. This column line and corresponding universal extraction method allows for excellent recoveries of both naturally occurring opiates and various fentanyl analogues. Check out our newly developed method here.
8. Oral Fluid Analysis
It’s no surprise that oral fluid drug testing has gained recent popularity in forensic and clinical laboratories. Not only is it easier to acquire from a sample collection perspective, but also, it’s much less invasive when comparing the measures utilized to solicit urine and blood samples. In addition, it’s much more difficult to adulterate. While there are several advantages when working with this matrix, oral fluid does have several drawbacks including lower drug concentrations, limited sample volume and preservative buffers that not only dilute the oral fluid sample but also cause ion suppression if not removed properly prior to analysis. UCT’s Clean-Screen® XCEL I solid phase extraction columns and methodology allow for a quick, efficient clean-up of oral-fluid samples providing excellent recoveries for acidic, neutral, and basic drugs in a concentrated format.
9. Synthetic Cannabinoid Analysis
The number of products marketed as “legal alternatives to cannabis” or “legal highs” have dramatically increased in popularity in recent years. It can be a real challenge for testing labs to keep up with the new, synthetic cannabinoids. Although these compounds are ever-changing, they are derived from “template structures”, which are ideal candidates for clean-up via solid phase extraction (SPE). Having a method that can not only target current metabolites of interest, but also the new ones being synthesized is key in order for laboratories to keep up with the constantly evolving market. Utilizing UCT’s SSHLD® extraction column and corresponding methodology allows for both THC and synthetic cannabinoid levels to be monitored simultaneously, reducing analyst time and instrument time. Check out the method here.
10. Designer Benzodiazepine Analysis
Compared to other classes of drugs, benzodiazepine abuse is relatively uncommon. However, there has been an upward trend of using them along with other drugs, such as alcohol and opioids, in order to achieve an enhanced overall high. Similar to other commonly abused compounds, such as cannabinoids or amphetamines, “legal” alternatives have been developed for benzos as well in an attempt to bypass the controlled substances act. Traditional benzodiazepines primarily function as neutral analytes, however, there are some that have weakly basic functional groups allowing for ionization at a fixed pH. The Clean Screen® XCEL I column has the capability of simultaneously extracting neutral and basic compounds, while eliminating the need for time-consuming column conditioning and extensive solvent usage for sample cleanup. Check out the method here.
Coming Soon - QuEChERS Technique for Handling Post-Mortem Matrices
In 2003, the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method was developed as a way to improve conventional sample preparation for multi-residue pesticide analysis in a variety of difficult matrices. While the methodology was initially invented for the food testing industry, it has recently caught the attention of several other types of analytical laboratories including the post-mortem drug testing communities. The QuEChERS technique provides bench analysts with the answer to extracting a large number of analytes from problematic matrices such as, tissue, liver or decomposed blood samples that are often difficult to manipulate for solid-phase extraction. UCT’s variety of salt blends come pre-packed in several different formats allowing for increased sample throughput. Coming soon are various applications using this approach for post-mortem matricies