To evaluate the DanceSafe Complete Adulterant Screening Kit for Ecstasy with regard to its accura... more To evaluate the DanceSafe Complete Adulterant Screening Kit for Ecstasy with regard to its accuracy in identifying 3,4-methylenedioxymeth-amphetamine (MDMA) and methylenedioxyamphetamine (MDA) derivatives and its ability to detect certain contaminants. In part 1, 39 street-grade tablets purported to be MDMA were tested with the Marquis, Mecke, and Simon's reagents provided by the DanceSafe testing kit. The tablets then were submitted to gas chromatography-mass spectrometry for identification of active ingredients. In part II, seven known drugs of abuse were tested with the Marquis, Mecke, and Simon's reagents. These drugs were codeine, dextromethorphan, dihydrocodeine, ketamine, MDMA, morphine, and d-norpropoxyphene. The Marquis, Mecke, and Simon's reagents did not differentiate pure MDMA from adulterated forms. They lacked both sensitivity and specificity for the purpose of MDMA identification when tested by persons unfamiliar with these reagents. Also, experienced toxicologists using this unfamiliar procedure generated false-positive results. Neither the Marquis, Mecke, nor Simon's reagents should be used by the public for harm reduction purposes. These agents do not help identify pure MDMA tablets. Gas chromatography-mass spectrometry remains the most sensitive and specific testing method for identifying MDMA and its contaminants.
To evaluate the DanceSafe Complete Adulterant Screening Kit for Ecstasy with regard to its accura... more To evaluate the DanceSafe Complete Adulterant Screening Kit for Ecstasy with regard to its accuracy in identifying 3,4-methylenedioxymeth-amphetamine (MDMA) and methylenedioxyamphetamine (MDA) derivatives and its ability to detect certain contaminants. In part 1, 39 street-grade tablets purported to be MDMA were tested with the Marquis, Mecke, and Simon's reagents provided by the DanceSafe testing kit. The tablets then were submitted to gas chromatography-mass spectrometry for identification of active ingredients. In part II, seven known drugs of abuse were tested with the Marquis, Mecke, and Simon's reagents. These drugs were codeine, dextromethorphan, dihydrocodeine, ketamine, MDMA, morphine, and d-norpropoxyphene. The Marquis, Mecke, and Simon's reagents did not differentiate pure MDMA from adulterated forms. They lacked both sensitivity and specificity for the purpose of MDMA identification when tested by persons unfamiliar with these reagents. Also, experienced toxicologists using this unfamiliar procedure generated false-positive results. Neither the Marquis, Mecke, nor Simon's reagents should be used by the public for harm reduction purposes. These agents do not help identify pure MDMA tablets. Gas chromatography-mass spectrometry remains the most sensitive and specific testing method for identifying MDMA and its contaminants.
... 1,1,2-TRICHLOROCYCLOALKANES Alan B. Brownl* Chris W. Chronister, Diana M. Watkins, Richard J.... more ... 1,1,2-TRICHLOROCYCLOALKANES Alan B. Brownl* Chris W. Chronister, Diana M. Watkins, Richard J. Mazzaccaro, Scott R. Rajski, Martha G. ... also run; 50-MHz 13C NMR spectra were obtained on a Va-rian Gemini 200 spectrometer. Detailed assignments were ...
A simple method for the direct analysis of gamma-hydroxybutyrate (GHB) from human urine is descri... more A simple method for the direct analysis of gamma-hydroxybutyrate (GHB) from human urine is described. The method uses solid-phase extraction, liquid-liquid extraction, and silyl-derivatization, then gas chromatographic-mass spectrometric analysis using GHB-d6 as the internal standard. The method was linear from 5 to 500 mg/L, and coefficients of variation were less than 10%. Twenty-six urine specimens previously analyzed by an existing method were analyzed and yielded GHB concentrations ranging from 0 to 6100 mg/L; the results correlated between the two methods. Compared with existing methods, the method described here is superior because it is specific to GHB and can discriminate between GHB and gamma-butyrolactone.
Synthetic cathinones are an emerging class of designer drugs, frequently with deceptive labels an... more Synthetic cathinones are an emerging class of designer drugs, frequently with deceptive labels and a multitude of analogs to circumvent drug control regulations. Research regarding the pharmacological effects and toxicity of these amphetamine derivatives is scarce, heightening the risk to the public health and safety. The composition of synthetic cathinone products continually changes and laboratories began to notice ethylone-positive products in late 2011. This report presents nine postmortem cases in whom ethylone was identified. Ethylone was isolated using solid-phase extraction and detected by gas chromatography-mass spectrometry. Seven of the cases had measurable concentrations of ethylone in blood, ranging from 38 to 2,572 ng/mL; ethylone was detected in the blood sample of one case with a concentration below the assay limit of quantification (25 ng/mL), and one case did not have detectable ethylone in blood. Besides ethylone, all but one case were also positive for 11-nor-9-c...
Methods in molecular biology (Clifton, N.J.), 2010
The opioid and 6-acetylmorphine assays utilize gas chromatography-mass spectrometry (GC-MS) for t... more The opioid and 6-acetylmorphine assays utilize gas chromatography-mass spectrometry (GC-MS) for the analysis of morphine, codeine, hydromorphone, hydrocodone, and 6-acetylmorphine in blood and urine. The specimens are fortified with deuterated internal standard and a five-point calibration curve is constructed. Specimens are extracted by mixed-mode solid phase extraction. The morphine, codeine, hydromorphone, hydrocodone, and 6-acetylmorphine extracts are derivatized with N-methyl-bis(trifluoroacetamide) (MBTFA) producing trifluoroacetyl derivatives. The final extracts are then analyzed using selected ion monitoring GC-MS.
Methods in molecular biology (Clifton, N.J.), 2010
Fentanyl is a potent, short-acting synthetic opioid analgesic. Fentanyl is measured in blood and ... more Fentanyl is a potent, short-acting synthetic opioid analgesic. Fentanyl is measured in blood and urine following mixed-mode solid phase extraction. The specimens are fortified with deuterated internal standard and a five-point calibration curve is constructed. The final extracts are reconstituted in methanol and analyzed using selected ion monitoring gas chromatography-mass spectrometry.
Methods in molecular biology (Clifton, N.J.), 2010
The benzodiazepine assay utilizes gas chromatography-mass spectrometry (GC-MS) for the analysis o... more The benzodiazepine assay utilizes gas chromatography-mass spectrometry (GC-MS) for the analysis of diazepam, nordiazepam, oxazepam, temazepam, lorazepam, alpha-hydroxyalprazolam, and alpha-hydroxytriazolam in blood and urine. A separate assay is employed for the analysis of alprazolam. Prior to solid phase extraction, urine specimens are subjected to enzyme hydrolysis. The specimens are fortified with deuterated internal standard and a five-point calibration curve is constructed. Specimens are extracted by mixed-mode solid phase extraction. The benzodiazepine extracts are derivatized with N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSFTA) producing tert-butyldimethyl silyl derivatives; the alprazolam extracts are reconstituted in methanol without derivatization. The final extracts are then analyzed using selected ion monitoring GC-MS.
Testing for drugs of abuse in urine is commonplace in emergency departments and neonatal units. H... more Testing for drugs of abuse in urine is commonplace in emergency departments and neonatal units. However, the clinical sensitivity of immunochemical screening methods is limited by the threshold concentrations used to distinguish between positive and negative specimens. Immunochemical screening methods for cocaine metabolite (benzoylecgonine), cannabinoids, and opiates in urine were recalibrated to detect drugs at lower threshold concentrations. The precision and linearity of the signals at the modified thresholds were verified by diluting drug-positive urine specimens to concentrations below the conventional cutoff concentration and measuring the rate signals in triplicate. To assess the clinical performance of the modified methods, specimens that tested negative using the unmodified assays were re-screened at the lower threshold, and specimens that re-screened positive were submitted for gas chromatographic/mass spectrometric (GC/MS) confirmation. Reproducibility of sub-threshold m...
To evaluate the DanceSafe Complete Adulterant Screening Kit for Ecstasy with regard to its accura... more To evaluate the DanceSafe Complete Adulterant Screening Kit for Ecstasy with regard to its accuracy in identifying 3,4-methylenedioxymeth-amphetamine (MDMA) and methylenedioxyamphetamine (MDA) derivatives and its ability to detect certain contaminants. In part 1, 39 street-grade tablets purported to be MDMA were tested with the Marquis, Mecke, and Simon's reagents provided by the DanceSafe testing kit. The tablets then were submitted to gas chromatography-mass spectrometry for identification of active ingredients. In part II, seven known drugs of abuse were tested with the Marquis, Mecke, and Simon's reagents. These drugs were codeine, dextromethorphan, dihydrocodeine, ketamine, MDMA, morphine, and d-norpropoxyphene. The Marquis, Mecke, and Simon's reagents did not differentiate pure MDMA from adulterated forms. They lacked both sensitivity and specificity for the purpose of MDMA identification when tested by persons unfamiliar with these reagents. Also, experienced toxicologists using this unfamiliar procedure generated false-positive results. Neither the Marquis, Mecke, nor Simon's reagents should be used by the public for harm reduction purposes. These agents do not help identify pure MDMA tablets. Gas chromatography-mass spectrometry remains the most sensitive and specific testing method for identifying MDMA and its contaminants.
To evaluate the DanceSafe Complete Adulterant Screening Kit for Ecstasy with regard to its accura... more To evaluate the DanceSafe Complete Adulterant Screening Kit for Ecstasy with regard to its accuracy in identifying 3,4-methylenedioxymeth-amphetamine (MDMA) and methylenedioxyamphetamine (MDA) derivatives and its ability to detect certain contaminants. In part 1, 39 street-grade tablets purported to be MDMA were tested with the Marquis, Mecke, and Simon's reagents provided by the DanceSafe testing kit. The tablets then were submitted to gas chromatography-mass spectrometry for identification of active ingredients. In part II, seven known drugs of abuse were tested with the Marquis, Mecke, and Simon's reagents. These drugs were codeine, dextromethorphan, dihydrocodeine, ketamine, MDMA, morphine, and d-norpropoxyphene. The Marquis, Mecke, and Simon's reagents did not differentiate pure MDMA from adulterated forms. They lacked both sensitivity and specificity for the purpose of MDMA identification when tested by persons unfamiliar with these reagents. Also, experienced toxicologists using this unfamiliar procedure generated false-positive results. Neither the Marquis, Mecke, nor Simon's reagents should be used by the public for harm reduction purposes. These agents do not help identify pure MDMA tablets. Gas chromatography-mass spectrometry remains the most sensitive and specific testing method for identifying MDMA and its contaminants.
To evaluate the DanceSafe Complete Adulterant Screening Kit for Ecstasy with regard to its accura... more To evaluate the DanceSafe Complete Adulterant Screening Kit for Ecstasy with regard to its accuracy in identifying 3,4-methylenedioxymeth-amphetamine (MDMA) and methylenedioxyamphetamine (MDA) derivatives and its ability to detect certain contaminants. In part 1, 39 street-grade tablets purported to be MDMA were tested with the Marquis, Mecke, and Simon's reagents provided by the DanceSafe testing kit. The tablets then were submitted to gas chromatography-mass spectrometry for identification of active ingredients. In part II, seven known drugs of abuse were tested with the Marquis, Mecke, and Simon's reagents. These drugs were codeine, dextromethorphan, dihydrocodeine, ketamine, MDMA, morphine, and d-norpropoxyphene. The Marquis, Mecke, and Simon's reagents did not differentiate pure MDMA from adulterated forms. They lacked both sensitivity and specificity for the purpose of MDMA identification when tested by persons unfamiliar with these reagents. Also, experienced toxicologists using this unfamiliar procedure generated false-positive results. Neither the Marquis, Mecke, nor Simon's reagents should be used by the public for harm reduction purposes. These agents do not help identify pure MDMA tablets. Gas chromatography-mass spectrometry remains the most sensitive and specific testing method for identifying MDMA and its contaminants.
... 1,1,2-TRICHLOROCYCLOALKANES Alan B. Brownl* Chris W. Chronister, Diana M. Watkins, Richard J.... more ... 1,1,2-TRICHLOROCYCLOALKANES Alan B. Brownl* Chris W. Chronister, Diana M. Watkins, Richard J. Mazzaccaro, Scott R. Rajski, Martha G. ... also run; 50-MHz 13C NMR spectra were obtained on a Va-rian Gemini 200 spectrometer. Detailed assignments were ...
A simple method for the direct analysis of gamma-hydroxybutyrate (GHB) from human urine is descri... more A simple method for the direct analysis of gamma-hydroxybutyrate (GHB) from human urine is described. The method uses solid-phase extraction, liquid-liquid extraction, and silyl-derivatization, then gas chromatographic-mass spectrometric analysis using GHB-d6 as the internal standard. The method was linear from 5 to 500 mg/L, and coefficients of variation were less than 10%. Twenty-six urine specimens previously analyzed by an existing method were analyzed and yielded GHB concentrations ranging from 0 to 6100 mg/L; the results correlated between the two methods. Compared with existing methods, the method described here is superior because it is specific to GHB and can discriminate between GHB and gamma-butyrolactone.
Synthetic cathinones are an emerging class of designer drugs, frequently with deceptive labels an... more Synthetic cathinones are an emerging class of designer drugs, frequently with deceptive labels and a multitude of analogs to circumvent drug control regulations. Research regarding the pharmacological effects and toxicity of these amphetamine derivatives is scarce, heightening the risk to the public health and safety. The composition of synthetic cathinone products continually changes and laboratories began to notice ethylone-positive products in late 2011. This report presents nine postmortem cases in whom ethylone was identified. Ethylone was isolated using solid-phase extraction and detected by gas chromatography-mass spectrometry. Seven of the cases had measurable concentrations of ethylone in blood, ranging from 38 to 2,572 ng/mL; ethylone was detected in the blood sample of one case with a concentration below the assay limit of quantification (25 ng/mL), and one case did not have detectable ethylone in blood. Besides ethylone, all but one case were also positive for 11-nor-9-c...
Methods in molecular biology (Clifton, N.J.), 2010
The opioid and 6-acetylmorphine assays utilize gas chromatography-mass spectrometry (GC-MS) for t... more The opioid and 6-acetylmorphine assays utilize gas chromatography-mass spectrometry (GC-MS) for the analysis of morphine, codeine, hydromorphone, hydrocodone, and 6-acetylmorphine in blood and urine. The specimens are fortified with deuterated internal standard and a five-point calibration curve is constructed. Specimens are extracted by mixed-mode solid phase extraction. The morphine, codeine, hydromorphone, hydrocodone, and 6-acetylmorphine extracts are derivatized with N-methyl-bis(trifluoroacetamide) (MBTFA) producing trifluoroacetyl derivatives. The final extracts are then analyzed using selected ion monitoring GC-MS.
Methods in molecular biology (Clifton, N.J.), 2010
Fentanyl is a potent, short-acting synthetic opioid analgesic. Fentanyl is measured in blood and ... more Fentanyl is a potent, short-acting synthetic opioid analgesic. Fentanyl is measured in blood and urine following mixed-mode solid phase extraction. The specimens are fortified with deuterated internal standard and a five-point calibration curve is constructed. The final extracts are reconstituted in methanol and analyzed using selected ion monitoring gas chromatography-mass spectrometry.
Methods in molecular biology (Clifton, N.J.), 2010
The benzodiazepine assay utilizes gas chromatography-mass spectrometry (GC-MS) for the analysis o... more The benzodiazepine assay utilizes gas chromatography-mass spectrometry (GC-MS) for the analysis of diazepam, nordiazepam, oxazepam, temazepam, lorazepam, alpha-hydroxyalprazolam, and alpha-hydroxytriazolam in blood and urine. A separate assay is employed for the analysis of alprazolam. Prior to solid phase extraction, urine specimens are subjected to enzyme hydrolysis. The specimens are fortified with deuterated internal standard and a five-point calibration curve is constructed. Specimens are extracted by mixed-mode solid phase extraction. The benzodiazepine extracts are derivatized with N-methyl-N-(tert-butyldimethylsilyl)trifluoroacetamide (MTBSFTA) producing tert-butyldimethyl silyl derivatives; the alprazolam extracts are reconstituted in methanol without derivatization. The final extracts are then analyzed using selected ion monitoring GC-MS.
Testing for drugs of abuse in urine is commonplace in emergency departments and neonatal units. H... more Testing for drugs of abuse in urine is commonplace in emergency departments and neonatal units. However, the clinical sensitivity of immunochemical screening methods is limited by the threshold concentrations used to distinguish between positive and negative specimens. Immunochemical screening methods for cocaine metabolite (benzoylecgonine), cannabinoids, and opiates in urine were recalibrated to detect drugs at lower threshold concentrations. The precision and linearity of the signals at the modified thresholds were verified by diluting drug-positive urine specimens to concentrations below the conventional cutoff concentration and measuring the rate signals in triplicate. To assess the clinical performance of the modified methods, specimens that tested negative using the unmodified assays were re-screened at the lower threshold, and specimens that re-screened positive were submitted for gas chromatographic/mass spectrometric (GC/MS) confirmation. Reproducibility of sub-threshold m...
To evaluate the DanceSafe Complete Adulterant Screening Kit for Ecstasy with regard to its accura... more To evaluate the DanceSafe Complete Adulterant Screening Kit for Ecstasy with regard to its accuracy in identifying 3,4-methylenedioxymeth-amphetamine (MDMA) and methylenedioxyamphetamine (MDA) derivatives and its ability to detect certain contaminants. In part 1, 39 street-grade tablets purported to be MDMA were tested with the Marquis, Mecke, and Simon's reagents provided by the DanceSafe testing kit. The tablets then were submitted to gas chromatography-mass spectrometry for identification of active ingredients. In part II, seven known drugs of abuse were tested with the Marquis, Mecke, and Simon's reagents. These drugs were codeine, dextromethorphan, dihydrocodeine, ketamine, MDMA, morphine, and d-norpropoxyphene. The Marquis, Mecke, and Simon's reagents did not differentiate pure MDMA from adulterated forms. They lacked both sensitivity and specificity for the purpose of MDMA identification when tested by persons unfamiliar with these reagents. Also, experienced toxicologists using this unfamiliar procedure generated false-positive results. Neither the Marquis, Mecke, nor Simon's reagents should be used by the public for harm reduction purposes. These agents do not help identify pure MDMA tablets. Gas chromatography-mass spectrometry remains the most sensitive and specific testing method for identifying MDMA and its contaminants.
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