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Biomedical subjects

K G Johnson

Publications and source records attributed to K G Johnson.

At least 127 records · Page 7Linked to original sources

Full spectral GC/MS identification of delta 9-carboxy-tetrahydrocannabinol in urine with the Finnigan ITS40.

The Finnigan MAT ITS40 GC/MS permits the accurate full mass spectral identification and reproducible quantitation of 11-nor-9-carboxy-delta 9-tetrahydrocannabinol (9-carboxy-THC) in urine. Positive identification of 9-carboxy-THC is based on full mass spectral cutoff criteria whose fit value is 900. The fit value is generated from a statistically significant correlation comparison of the targeted unknown against an authentic 9-carboxy-THC standard, whose mass spectrum has been generated on the ITS40. The limit of detection (LOD) and limit of quantitation (LOQ) are 2.5 ng/mL and 5 ng/mL, respectively, using 5 mL of urine. The quantitative linear dynamic range of the assay is greater than two orders of magnitude, ranging from 5 to 1,000 ng/mL.

Dronabinol↗

Alcohol-specific cocaine metabolites in serum and urine of hospitalized patients.

The serum and urine from 44 consecutive patients that tested positive for the cocaine metabolite benzoylecgonine (BE) were examined for free cocaine, ecgonine methyl ester (EME), and other metabolites by gas chromatography/ion trap mass spectrometry (GC/MS). In 13 of these patients, unique ethanol-related cocaine metabolites, cocaethylene and ecognine ethyl ester (EEE), were detected in urine and serum. One was from a newborn baby whose mother's blood was positive for cocaine and negative for cocaethylene. In two other patients, isopropanol was also consumed with cocaine and ethanol. In one of these two, cocaisopropylene and ecognine isopropyl ester (EPE) were identified in urine. The urine ethanol concentration in 7 of the 13 cocaethylene-positive patients ranged from 19 to 322 mg/dL. In the other six, ethanol was not detected in the urine. However, each of these latter patients had either prior serum results that were positive for ethanol or admitted to recent alcohol abuse. In the remaining 31 of 44 cocaine-positive patients, ethanol and the alcohol-specific cocaine metabolites were absent. The detection of alcohol-related cocaine metabolites is fairly common in a cocaine-positive patient population.

Adult↗

Identification of methamphetamines and over-the-counter sympathometic amines by full-scan GC-ion trap MS with electron impact and chemical ionization.

An underivatized methane chemical ionization (CI) assay for measuring amphetamines in urine was evaluated against derivatized electron impact (EI) assays using a gas chromatograph-ion trap mass spectrometer. The full-scan CI mass spectra of methamphetamine, ephedrine/pseudoephedrine, and phentermine were compared with the full scan and three-ion EI mass spectra of heptafluorobutyric anhydride (HFBA) and 4-carbethoxyhexafluorobutyryl chloride (CB) derivatives. The fragmentation patterns for these compounds were nearly identical for the three major high molecular weight ions (m/z 254, 210, and 169 for EI-HFBA derivatives, and m/z 308, 262, and 280 for EI-CB derivatives). The CI mass spectra of the underivatized drugs contained more discernible differences at the higher molecular weights, including m/z 119, 148, and 150 for methamphetamine, 148, 166, and 176 for ephedrine/pseudoephedrine, and 91, 133, and 150 for phentermine. The within-run precision ranged from 7-9% for CI versus 5-6% for EI with HFBA derivatization (mean 500 ng/mL, n = 5). The limits of detection (LOD) for amphetamine and methamphetamine were 2.4 and 8.6 ng/mL, respectively, for CI versus 0.7 and 1.4 ng/mL for EI. The limits of quantitation (LOQ) were 4.5 and 19.1 ng/mL for CI versus 1.4 and 5.7 ng/mL for EI. The use of full-scan mass spectral analysis with either electron impact or chemical ionization provides additional qualitative data that may be helpful for measuring methamphetamine in the presence of other sympathomimetic amines.

Amphetamine↗

Evaluation of full-scanning GC/ion trap MS analysis of NIDA drugs-of-abuse urine testing in urine.

Analytical methods developed for the Finnigan MAT ITS40 gas chromatograph-ion trap mass spectrometer (GC/MS) were evaluated for the confirmation of drugs-of-abuse in urine. The specific drugs evaluated are those listed by the National Institute on Drug Abuse (NIDA): 11-nor-9-carboxy-delta 9-tetrahydrocannabinol (9-carboxy-THC), benzoylecgonine (BE), codeine and morphine, phencyclidine (PCP), amphetamine, and methamphetamine. Drugs were extracted from urine using solid-phase columns, separated by capillary gas chromatography, and analyzed by ion trap mass spectrometry following electron impact ionization. All drugs except PCP were derivatized prior to analysis. The full scan limits of detection (LOD), quantitation (LOQ), and linearity were 2.5, 5.0, and 1000 ng/mL, respectively, for 9-carboxy-THC; 37, 75, and 5000 ng/mL for BE; 50, 100, and 2500 ng/mL for the opiates; 0.25, 0.50, and 500 ng/mL for PCP; and 50, 100, and 5000 ng/mL for the amphetamines. The limits of detection (LOD) and limits of quantitation (LOQ) met the minimum criteria for the signal-to-noise (S/N) ratio and spectral match criteria for drug identification. Absolute LODs and LOQs (in ng/mL) for the ITS40 based on single ion monitoring of blank urines were: 0.8 and 2.0 for 9-carboxy-THC; 8.9 and 25 for BE; 3.3 and 9.6 for codeine; 6.2 and 16.7 for morphine; 0.25 and 0.32 for PCP; 0.7 and 2.0 for amphetamine; and 2.4 and 5.7, for methamphetamine, respectively. The coefficient of variation ranged from 5 to 10%, and analytical recoveries were in the range of 90-114%. The ion trap mass spectrometer permits full scan identification of drugs while maintaining analytical LOQ that are below NIDA guidelines, and has equivalent or better detection limits to quadrupole analyzers for high sensitivity applications.

Evaluation Studies as Topic↗

Extraction and simultaneous elution and derivatization of 11-nor-9-carboxy-delta 9-tetrahydrocannabinol using Toxi-Lab SPEC prior to GC/MS analysis of urine.

A new sample preparation procedure is described for the extraction and simultaneous elution and derivation of urine for analysis of 11-nor-9-carboxy-delta 9-tetrahydrocannabinol (THC-COOH) by gas chromatography/ion trap mass spectrometry (GC/MS). Urine samples are extracted for THC-COOH and d6-THC-COOH internal standard onto a hydrophobic membrane. Extracts are simultaneously eluted and derivatized with MSTFA while on the membrane to produce the corresponding trimethylsilane derivative. Using results of blank urine, the limits of detection and quantitation were 1.1 and 2.5 ng/mL, respectively. The linearity of the assay was 250 ng/mL. The within-run and day-to-day precision ranged 3-5%. Compared with a solid-phase column extraction procedure, the overall time for sample preparation was decreased from 3 h down to 1. The SPEC extraction procedure with trimethyl derivatization produces a cleaner total ion chromatogram than the solid-phase column extraction system (minicolumn) and does not require the use of any organic solvents.

Dronabinol↗

Evaluation of the triage system for emergency drugs-of-abuse testing in urine.

The Triage Panel for Drugs of Abuse (DOA) was evaluated for detection of phencyclidine (PCP), amphetamines (AMPH), opiates (OPI), tetrahydrocannabinol (THC), the cocaine metabolite benzoylecgonine (BE), and barbiturates (BARB) in urine. This assay was compared with Syva EMIT. The comparisons were conducted on 606 positive and 325 negative samples. When there was a sufficient volume of sample available for retesting, positive and negative samples with discordant results between these two screening assays were confirmed by quantitative gas chromatography/mass spectrometry (GC/MS). The percent agreement between the two assays for positive samples ranged from 93 to 100%. For negative samples, the agreement ranged from 95 to 100%. For AMPH, 19 out of 27 discordant samples of urine that were positive for EMIT and negative for Triage DOA contained total amphetamine and methamphetamine concentrations of less than 1000 ng/mL by GC/MS. For THC, seven urine samples that were negative for Triage DOA and positive for EMIT contained 9-carboxy THC concentrations at greater than 15 ng/mL by GC/MS. For BARB, three samples that were negative for Triage DOA and positive for EMIT contained barbiturates levels greater than 300 ng/mL. Two of these three samples contained phenobarbital below the concentration that produces a positive result for Triage DOA. For the majority of the urine samples studied, however, the Triage DOA produced identical results to a commercial-instrument-based immunoassay.

Emergencies↗