Lactose is commonly used as a cutting agent in illicit drugs. Currently, presumptive field color test kits for illicit drugs do not test for the presence of lactose or other cutting agents. A method was developed to detect lactose on a paper-based test card. A three-enzyme system comprised of lactase, glucose oxidase, and peroxidase was used to break down lactose into peroxide, which was then detected with a redox indicator. The test can detect lactose concentrations as low as 5% in solid samples and shows no interference when lactose is mixed with illicit drugs or commercial pharmaceuticals. Prepared test cards were stable on the shelf for up to five months. In a blinded study of samples composed of mixtures of heroin, methamphetamine, cocaine HCl, crack cocaine, fillers, and lactose, the sensitivity for detection of lactose across three readers was 100% and specificity was 96.4% ( n = 96). When this test was incorporated into a 12-lane test card for the detection of illicit drugs, readers were correctly able to identify the illicit drug and the presence of lactose with 99.3% sensitivity and 100% specificity ( n = 54). This test is a robust and affordable way to detect lactose in illicit drug samples.
more »
« less
Assessing Hair Decontamination Protocols for Diazepam, Heroin, Cocaine and Δ9-Tetrahydrocannabinol by Statistical Design of Experiments
Abstract Prior to toxicological analysis, hair as a matrix requires pre-treatment measures including decontamination, homogenization and extraction. Decontamination is performed to differentiate between drug present from superficial deposition and drug incorporated from systemic distribution following ingestion. There are many methods for decontamination of hair samples, mostly developed by empirically using a traditional “one factor at a time” approach, in which one independent variable at a time is changed to observe the effect on the dependent variable. The goal of the present work was to compare the efficacy of decontamination protocols using statistical “design of experiments” (DoE), which allows for analysis of multiple variables and interactions within a single experiment. Decontamination parameters included identity of aqueous and organic wash solutions, number of sequential aqueous and organic washes, order of aqueous and organic washes, and duration of each wash. DoE studies were completed to identify optimal decontamination conditions for four abused drugs with varying physiochemical properties. For this purpose, drug-free human hair was externally contaminated with diazepam, heroin, cocaine or Δ9-tetrahydrocannabinol. Each analyte was found to have a unique set of decontamination conditions that were most effective. These included three 30-min washes with methanol followed by three with 1% sodium dodecyl sulfide for diazepam, three 30-s washes with dichloromethane followed by one with water for heroin, one 30-s wash with 1% sodium dodecyl sulfate followed by three with dichloromethane for cocaine and three 30-min washes with water followed by one with methanol for Δ9-tetrahydrocannabinol. The results provide proof-of-principle for a DoE approach to identify effective parameters for hair decontamination for a physicochemically diverse group of drugs. The major advantage of DoE is to elucidate combinations of parameters that result in effective removal of surface contamination, a goal that would be challenging to accomplish using a one factor at a time approach.
more »
« less
- Award ID(s):
- 1739805
- PAR ID:
- 10235038
- Date Published:
- Journal Name:
- Journal of Analytical Toxicology
- Volume:
- 45
- Issue:
- 5
- ISSN:
- 0146-4760
- Page Range / eLocation ID:
- 498 to 505
- Format(s):
- Medium: X
- Sponsoring Org:
- National Science Foundation
More Like this
-
-
A water-soluble host molecule can bind tetrahydrocannabinol ( Δ9-THC ) and its metabolites in aqueous solution. By pairing this recognition event in a sensing array with fluorescent reporters and varying external mediators, pattern recognition-based detection is possible, which allows selective discrimination of the THC metabolites. The selective sensing can be performed in aqueous solution with micromolar sensitivity, as well as in biofluids such as urine and saliva. Metabolites as similar as Δ8- and Δ9-THC , differing only in the position of a double bond, can be distinguished.more » « less
-
Recently there has been upsurge in reports that illicit seizures of cocaine and heroin have been adulterated with fentanyl. Surface-enhanced Raman spectroscopy (SERS) provides a useful alternative to current screening procedures that permits detection of trace levels of fentanyl in mixtures. Samples are solubilized and allowed to interact with aggregated colloidal nanostars to produce a rapid and sensitive assay. In this study, we present the quantitative determination of fentanyl in heroin and cocaine using SERS, using a point-and-shoot handheld Raman system. Our protocol is optimized to detect pure fentanyl down to 0.20 ± 0.06 ng/mL and can also distinguish pure cocaine and heroin at ng/mL levels. Multiplex analysis of mixtures is enabled by combining SERS detection with principal component analysis and super partial least squares regression discriminate analysis (SPLS-DA), which allow for the determination of fentanyl as low as 0.05% in simulated seized heroin and 0.10% in simulated seized cocaine samples.more » « less
-
After attending this presentation, attendees will gain knowledge in the strategy to achieve high-throughput and simultaneous analysis of cannabinoids and appreciate a validated LC-UV method for analysis of twelve cannabinoids in hemp oil. This presentation will first impact the forensic science community by introducing three fast LC separations of twelve cannabinoids that can be used with either UV or mass spectrometric (MS) detection. It will further impact the forensic science community by introducing a validated LC-UV method for high-throughput and simultaneous analysis of twelve cannabinoids in hemp oil, which can be routinely used by cannabis testing labs. In recent years, the use of products of Cannabis sativa L. for medicinal purposes has been in a rapid growth, although their preparation procedure has not been clearly standardized and their quality has not been well regulated. To analyze the therapeutic components, i.e. cannabinoids, in products of Cannabis sativa L., LC-UV has been frequently used, because LC-UV is commonly available and usually appropriate for routine analysis by the cannabis growers and commercial suppliers. In the literature, a few validated LC-UV methods have been described. However, so far, all validated LC-UV methods only focused in the quantification of eleven or less cannabinoids. Therefore, a method able to simultaneously analyze more cannabinoids in a shorter run time is still in high demand, because more and more cannabinoids have been isolated and many of them have shown medicinal properties. In this study, the LC separation of twelve cannabinoids, including cannabichromene (CBC), cannabidiolic acid (CBDA), cannabidiol (CBD), cannabidivarinic acid (CBDVA), cannabidivarin (CBDV), cannabigerolic acid (CBGA), cannabigerol (CBG), cannabinol (CBN), delta-8 tetrahydrocannabinol (Δ8-THC), delta-9 tetrahydrocannabinolic acid A (Δ9-THCA A), delta-9 tetrahydrocannabinol (Δ9-THC), and tetrahydrocannabivarin (THCV), has been systematically optimized using a Phenomenex Luna Omega 3 µm Polar C18 150 mm × 4.6 mm column with regard to the effects of the type of organic solvent, i.e. methanol and acetonitrile, the content of the organic solvent, and the pH of the mobile phase. The optimization has resulted in three LC conditions at 1.0 mL/minute able to separate the twelve cannabinoids: 1) a mobile phase consisting of water and methanol, both containing 0.1% formic acid (pH 2.69), with a gradient elution at 75% methanol for the first 3 minutes and then linearly increase to 100% methanol at 12.5 minutes; 2) a mobile phase consisting of water and 90% (v/v) acetonitrile in water, both containing 0.1% formic acid and 20 mM ammonium formate (pH 3.69), with an isocratic elution at 75% acetonitrile for 14 minutes; and 3) a mobile phase consisting of water and 90% (v/v) acetonitrile in water, both containing 0.03% formic acid and 20 mM ammonium formate (pH 4.20), with an isocratic elution at 75% acetonitrile for 14 minutes. In order to demonstrate the effectiveness of the achieved LC separations, a LC-UV method is further validated for the high-throughput and simultaneous analysis of twelve cannabinoids. The method used the mobile phase at pH 3.69, which resulted in significant improvement in throughput compared to other validated LC-UV methods published so far. The method used flurbiprofen as the internal standard. The linear calibration range of all the cannabinoids were between 0.1 to 25 ppm with R2≥0.9993. The LOQ (S/N=10) of the cannabinoids was between 17.8 and 74.2 ppb. The validation used a hemp oil containing 3.2 wt% CBD and no other cannabinoids, which was reported by the vendor with a certificate of analysis, as the matrix to prepare control samples: the hemp oil was first extracted using liquid-liquid extraction (LLE) with methanol; cannabinoids were then spiked into the extract at both 0.5 ppm and 5 ppm level. Afterwards, the recovery, precision (%RSD) and accuracy (%Error) of the control samples were assessed and the results met the requirements by the ISO/IEC 17025 and ASTM E2549-14 guidelines.more » « less
-
When synthetic polyamines, such poly(allylamine hydrochloride) (PAH), are mixed with crosslink-forming multivalent anions, they can undergo complex coacervation. This phenomenon has recently been exploited in various applications, ranging from inorganic material synthesis, to underwater adhesion, to multiple-month release of small, water-soluble molecules. Here, using ibuprofen as a model drug molecule, we show that these coacervates may be especially effective in the long-term release of weakly amphiphilic anionic drugs. Colloidal amphiphile/polyelectrolyte complex dispersions are first prepared by mixing the amphiphilic drug (ibuprofen) with PAH. Pentavalent tripolyphosphate (TPP) ions are then added to these dispersions to form ibuprofen-loaded PAH/TPP coacervates (where the strongly-binding TPP displaces the weaker-bound ibuprofen from the PAH amine groups). The initial ibuprofen/PAH binding leads to extremely high drug loading capacities (LC-values), where the ibuprofen comprises up to roughly 30% of the coacervate mass. Conversely, the dense ionic crosslinking of PAH by TPP results in very slow release rates, where the release of ibuprofen (a small, water-soluble drug) is extended over timescales that exceed 6 months. When ibuprofen is replaced with strong anionic amphiphiles, however ( i.e. , sodium dodecyl sulfate and sodium dodecylbenzenesulfonate), the stronger amphiphile/polyelectrolyte binding disrupts PAH/TPP association and sharply increases the coacervate solute permeability. These findings suggest that: (1) as sustained release vehicles, PAH/TPP coacervates might be very attractive for the encapsulation and multiple-month release of weakly amphiphilic anionic payloads; and (2) strong amphiphile incorporation could be useful for tailoring PAH/TPP coacervate properties.more » « less
An official website of the United States government

