Testing for kavain in human hair using gas chromatography-tandem mass spectrometry.

A sensitive, specific and reproducible method for the quantitative determination of kavain in human hair has been developed. The sample preparation involved a decontamination step of the hair with methylene chloride. The hair sample (about 50 mg) was incubated in 1 ml of methanol for 1 h, in an ultrasonic bath, in presence of 20 ng of methaqualone-d7 used as internal standard. The methanolic solution was evaporated to dryness, and the residue reconstituted by adding 30 microl of methanol. A 2 microl aliquot of the extract was injected onto the column (Optima5-MS capillary column, 5% phenyl-95% methylsiloxane, 30 m x 0.25 mm i.d. x 0.25 mm film thickness) of a Hewlett-Packard (Palo Alto, CA) gas chromatograph (5890). Kavain was detected by its parent ion at m/z 230 and daughter ions at m/z 111 and 202 through a Finnigan TSQ 700 MS/MS system. The assay was capable of detecting 30 pg/mg of kavain (limit of detection (LOD)). Linearity was observed for kavain concentrations ranging from 100 to 2000 pg/mg with a correlation coefficient of 0.998. Intra-day precision at 400 pg/mg was 13.7%. The analysis of a segment of hair, obtained from an occasional consumer, revealed the presence of kavain at the concentration of 418 pg/mg. A higher concentration (1708 pg/mg) was detected in the corresponding pubic hair.

Sweat testing in opioid users with a sweat patch.

For many years, toxicologists have detected the presence of drugs of abuse in biological materials using blood or urine. In recent years, remarkable advances in sensitive analytical techniques have enabled the analysis of drugs in unconventional samples such as sweat. In a study conducted in a detoxification center, sweat patches were applied to 20 known heroin abusers. Subjects wore the patch with minimal discomfort for five days. During the same period, two urine specimens were also collected. Target drugs analyzed either by gas chromatography-mass spectrometry (GC-MS) or liquid chromatography-mass spectrometry (LC-MS) included opiates (heroin, 6-monoacetylmorphine, morphine, codeine), cocaine (cocaine, benzoylecgonine, ecgonine methyl ester), delta 9-tetrahydrocannabinol, benzodiazepines (nordiazepam, oxazepam), amphetamines (amphetamine, methamphetamine, methylenedioxyamphetamine [MDA], methylenedioxymethamphetamine [MDMA], methylenedioxyethylamphetamine [MDEA]), and buprenorphine. Patches were positive for opiates in 12 cases. Heroin (37-175 ng/patch) and/or 6-acetylmorphine (60-2386 ng/patch) were identified in eight cases, and codeine exposure (67-4018 ng/patch) was determined in four cases. When detected, heroin was always present in lower concentrations than 6-acetylmorphine, which was the major analyte found in sweat. Cocaine (324 ng/patch) and metabolites were found in only one case. delta 9-Tetrahydrocannabinol (4-38 ng/patch) was identified in nine cases. Benzodiazepine concentrations were very low, ranging from 2 to 44 and from 2 to 15 ng/patch for nordiazepam and oxazepam, respectively. MDEA (121 ng/patch) and its metabolite, MDA (22 ng/patch), were detected in one case. Buprenorphine, which was administered as therapy under close medical supervision, was detected in the range 1.3-153.2 ng/patch with no apparent relationship between the daily dose and amount excreted in sweat. All the urine tests were consistent with the sweat findings, but to identify the same drugs it was necessary to test two urine specimens along with only one sweat specimen. It was concluded that sweat testing appears to offer the advantage of being a relatively noninvasive means of obtaining a cumulative estimate of drug exposure over the period of a week. This new technology may find useful applications in the treatment and monitoring of substance abusers, as the patch provides a long-term continuous monitor of drug exposure or noncompliance.

Simultaneous determination of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine and 3,4-methylenedioxymethamphetamine in human hair by gas chromatography-mass spectrometry.

A procedure is presented for the simultaneous identification and quantification of amphetamine (AP), methamphetamine (MA), methylenedioxyamphetamine (MDA) and methylenedioxymethamphetamine (MDMA) in human hair. The method involves decontamination of hair with dichloromethane and warm water, heat-alkaline hydrolysis in the presence of deuterated internal standards, liquid-liquid extraction and gas chromatography-mass spectrometry after derivatization with pentafluoropropionic anhydride-pentafluoropropanol. The limit of detection for AP, MA and MDA was 0.05 ng/mg using a 50-mg hair sample; for MDMA it was 0.1 ng/mg. Coefficients of variation ranged from 7 to 18%. This assay has been successfully utilized in the evaluation of the deposition of the drugs in hair obtained from various parts of the anatomy of a stimulant abuser.

Characterization of dextromoramide (Palfium) abuse by hair analysis in a denied case.

By providing information on exposure to drugs over time, hair analysis is useful in verifying the history of drug use. In a clinical case, where drug abuse was denied, it was possible to identify dextromoramide in the hair of the subject. After acid hydrolysis of the hair with 0.1 M HCl, in the presence of SKF 525A as an internal standard, the drug was extracted at pH 8.4 with chloroform-isopropanol-n-heptane (50:17:33 v/v) and quantified by gas chromatography/mass spectrometry. The hair strands were cut into 3 sections of 2.5 cm, corresponding to a growth period of 2 months. Concentrations were 1.09, 1.93 and 1.48 ng/mg from the root to the end, respectively. This is the first report on dextromoramide testing in human hair.

[Tobacco, drug and narcotic abuse during pregnancy. Evaluation of in utero exposure by analysis of hair of the neonate]. / Tabac, médicaments et stupéfiants pendant la grossesse. Evaluation de l'exposition in utero par analyse des cheveux du nouveau-né.

Hair samples were collected at the time of delivery from 63 neonates whose mothers were known to be heroin (9 cases), nicotine (40 cases), benzodiazepines (11 cases), cocaine (2 cases) and amphetamine (1 case) users. In all cases, the corresponding drug was found in neonatal hair from the infants, with concentrations in the range 0.61-3.47 ng/mg (morphine), 0.15-11.80 ng/mg (nicotine), 3.36-17.55 ng/mg (diazepam), 0.78-31.83 ng/mg (oxazepam), 0.71-2.47 ng/mg (benzoylecgonine), and 1.21 ng/mg (amphetamine). A significant correlation (P < 0.001) was established between nicotine concentration in the hair of the neonates, and in the hair of their mother.

Determination of nalbuphine using high-performance liquid chromatography coupled to photodiode-array detection and gas chromatography coupled to mass spectrometry.

A procedure involving capillary column gas chromatography coupled to mass spectrometry and a method involving liquid chromatography coupled to a diode-array detector have been developed for the analysis of nalbuphine. The extraction step is the same for both techniques and involves extraction under alkaline conditions in chloroform-2-propanol-n-heptane (50:17:33, v/v/v) with levallorphan as the internal standard. After purification by acidic extraction and back alkaline extraction, drugs are derivatized with N,O-bis-(trimethylsilyl)trifluoroacetamide with 1% trimethylchlorosilane for gas chromatography-mass spectrometry and directly injected for high-performance liquid chromatography-diode-array detection. The limits of detection are 2.0 and 25.0 ng/mg, respectively.

Detection of drugs in human hair for clinical and forensic applications.

While hair has for sometime been analyzed for assessment of trace elements, it is only in recent years that attention has been focused on this matrix as a possible means of evaluating drug impregnation. This technique was applied to treated subjects and drug abusers for determination of drug consumation. The method involved decontamination in ethanol, solubilization in sodium hydroxide at 100 degrees C for 10 min, extraction in chloroform/isopropanol/n-heptane (50:17:33, v/v), separation on a BP-5 capillary column (GC) and detection by mass spectrometry. Hair samples were analysed for barbiturates, antidepressants, benzodiazepines, beta-blockers, nicotine, opiates, benzoylecgonine, cannabis and amphetamines.

Simultaneous screening and quantification of several nonopiate narcotic analgesics and phencyclidine in human plasma using capillary gas chromatography.

This paper describes a procedure for the quantitative determination of alfentanil, dextromoramide, fentanyl, methadone, pentazocine, pethidine, phenoperidine and phencyclidine in human plasma. Some drug metabolites were included in the study. The procedure involves a simple alkaline extraction technique and capillary gas chromatography separation followed by a nitrogen-selective detection. Concentrations as low as 10 micrograms/l can be routinely evaluated, making this method suitable for use in overdose drug screening, therapeutic drug monitoring and pharmacokinetic studies.

Simultaneous determination of dextropropoxyphene, norpropoxyphene and methaqualone in plasma by gas chromatography with selective nitrogen detection.

A method for the identification and quantification of dextropropoxyphene, norpropoxyphene, and methaqualone in plasma by GC/NPD is presented. The procedure employs cyclizine as the internal standard and requires no derivatization. After a single-step extraction, analysis is achieved in 8 min. The lower limits of detection were found to be 6, 12, and 1 ng/ml for dextropropoxyphene, norpropoxyphene, and methaqualone, respectively. This method appears to be rapid, sensitive, and applicable to forensic and clinical toxicological analyses.

A simple gas chromatographic identification and determination of 11 CNS stimulants in biological samples. Application on a fatality involving phendimetrazine.

A method is presented for the simultaneous identification and quantification of several CNS stimulants, including amphetamine in plasma and urine by GC/FID using mephentermine as an internal standard. No derivation is necessary and after a single alkaline extraction, GC analysis for the 11 compounds tested is achieved in 23 min. The lower limit of detectability was found to be 4 ng/ml for amphetamine in plasma. This method is sensitive, reproducible, selective and applicable in forensic and clinical toxicological analyses. Toxicological findings, after a fatality involving phendimetrazine are presented as an application of the procedure.