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Biomedical subjects

V Cirimele

Publications and source records attributed to V Cirimele.

At least 55 records · Page 3Linked to original sources
PubMed1997

Testing human hair for flunitrazepam and 7-amino-flunitrazepam by GC/MS-NCI.

To validate information on flunitrazepam use, we investigated human hair for flunitrazepam and its major metabolite 7-amino-flunitrazepam by gas chromatography coupled to mass spectrometry in negative chemical ionization mode of detection. Samples were twice decontaminated with methylene chloride, pulverized in a ball mill and 50 mg of powdered hair were incubated in Soerensen buffer (pH 7.6) in the presence of diazepam-d5 used as internal standard. After liquid-liquid extraction of the incubation medium with diethylether-chloroform (80:20, by vol.), the organic phase was evaporated and the dry extract was derivatizated with heptafluorobutyric anhydride. Benzodiazepines were separated on a 30 m capillary column and detected using single ion monitoring. Among 40 hair samples tested (obtained from drug addicts deceased by heroin overdose), 14 were positive for both flunitrazepam and 7-amino-flunitrazepam and 12 for 7-amino-flunitrazepam only. Concentrations ranged from 31 to 129 pg/mg (mean: 60 pg/mg) and from 3 to 161 pg/mg (mean: 46 pg/mg) for flunitrazepam (14 cases) and 7-amino-flunitrazepam (26 cases), respectively. This first report described the detection of flunitrazepam and 7-amino-flunitrazepam in hair of chronic abusers. Due to the low concentrations observed, negative chemical ionization appears to be the alternative to test flunitrazepam and other benzodiazepines in hair.

Flunitrazepam↗
PubMed1997

Evidence of crack use by anhydroecgonine methylester identification.

A method using gas chromatography coupled to mass spectrometry for the determination of cocaine (COC) pyrolysis product, anhydroecgonine methylester (AEME), in plasma, saliva, urine, sweat and hair is described. The same procedure allows the simultaneous determination of COC, benzoylecgonine (BZE), ecgonine methylester (EME) and cocaethylene (CE). After suitable sample preparation (desorption of the sweat patch, acid hydrolysis of the hair) the target drugs were extracted using a 3-steps liquid-liquid extraction (pH 8.4) in presence of deuterated internal standards in chloroform-isopropanol-n-heptane (50 : 17 : 33, v/v). Derivatization was achieved using BSTFA+1% TMCS. Ions for AEME monitoring were m/z 82, 166, 152 and 181. Artifact formation from COC or EME of AEME during the injection was less than 0.5%. AEME was never detected in blood sample although the corresponding urine tested positive. Urine concentrations, in about 90 positive AEME samples, were in the range 5 to 1477 ng/ml. In one case of crack overdose, AEME in sweat was 53 ng/patch with a COC concentration of 1231 ng/patch. AEME in saliva ranged from 5 to 18 ng/ml in the same case. Finally, AEME was identified in 32 hair specimens of crack abusers including fetal hair, with concentrations in the range 0.20 to 21.56 ng/mg. These results suggest that AEME can be a useful marker for the detection of COC smoking in clinical and forensic cases.

Cocaine↗
PubMed1997

Enantioselective separation of methadone and its main metabolite in human hair by liquid chromatography/ion spray-mass spectrometry.

Optical isomers exhibit significant differences in their affinities for receptor sites, biotransformation and binding to serum and tissue proteins. Methadone has been used for the substitution of heroin addicts since 1964. The racemic form is used, i.e., a mixture of the biologically active R-form and the practically inactive S-form. To investigate methadone distribution, a chiral separation of the isomers was developed in human hair samples. The method involves decontamination of hair with water and acetone, pulverization in a ball mill, enzymatic hydrolysis in presence of deuterated internal standards, solid-phase extraction, and liquid chromatography/ion spray-mass spectrometry. Enantioselective separation of methadone and its main metabolite, EDDP, was obtained using an alpha1-acid glycoprotein column (100 by 4 mm ID). In all nine specimens obtained from subjects under racemic methadone treatment in a detoxification center, R- and S-enantiomers of methadone and EDDP were identified with the following concentrations: 2.58-10.22, 1.89-9.53, 0.42-1.73, and 0.40-2.10 ng/mg for R-methadone, S-methadone, R-EDDP, and S-EDDP, respectively. Results are suggestive of a predominance of the Renantiomer of methadone in human hair.

Chromatography, Liquid↗
PubMed1996

Hair analysis for nordiazepam and oxazepam by gas chromatography--negative-ion chemical ionization mass spectrometry.

A procedure is presented for the identification of nordiazepam and its metabolite, oxazepam, in human hair. The method involves decontamination of hair with dichloromethane, incubation in phosphate buffer (pH 7.6) in the presence of deuterated internal standards, liquid-liquid extraction, derivatization with N,O-bis(trimethylsilyl)trifluoroacetamide plus 1% trimethylchlorosilane and gas chromatography-mass spectrometry using negative-ion chemical ionization with methane. Among thirty samples obtained from polydrug abusers, thirteen tested positive for nordiazepam, in the range of 0.25-18.87 ng/mg. Five samples were also positive for oxazepam, in the range 0.11-0.50 ng/mg.

Adult↗
PubMed1996

Detection and quantification of lorazepam in human hair by GC-MS/NCI in a case of traffic accident.

A traffic accident caused by a man who declared that he was driving under influence of drugs (Temesta), led our laboratory to develop a procedure for the detection and the quantification of lorazepam in human hair. The method involves decontamination of hair with dichloromethane, incubation in Soerensen buffer (pH 7.6) in the presence of lorazepam-d4, liquid-liquid extraction with diethylether-chloroform (80:20, v/v) at pH 8.4, derivatization by silylation and detection by GC-MS/NCI. The increasing concentrations of lorazepam from the end to the roots of a 16-cm-long hair strand (i.e. 31 pg/mg, 40 pg/mg and 49 pg/mg) proved that the driver had taken the drug over a long period of time.

Accidents, Traffic↗
PubMed1996

[Detection of nordiazepam in the hair of drug addicts].

Hair samples were obtained from 36 drug addicts deceased from fatal heroin overdose. Samples were decontaminated with dichloromethane and pulverized. 50 mg of powdered hair were incubated 2 h at 40 degrees C in a phosphate buffer pH 7.6 in presence of deuterated internal standards (Nordiazepam-d5 and Oxazepam-d5) and extracted by a mixture ether/chloroform (80:20, v/v) at pH 8.4. After evaporation of the solvent, the dry extract was derivatized by silylation (BSTFA + 1% TMCS) and analyzed by gas chromatography coupled to mass spectrometry, with a detector operating in negative chemical ionization mode. 13 samples tested positive for Nordiazepam with concentrations ranging from 0.25 to 18.87 ng/mg of hair (mean: 4.16 ng/mg) and 5 positives for its metabolite, Oxazepam, with concentrations ranging from 0.11 to 0.50 ng/mg of hair (mean : 0.28 ng/mg).

Gas Chromatography-Mass Spectrometry↗
PubMed1995

A fatal dothiepin overdose.

High pressure liquid chromatography coupled to photodiode array detector and capillary gas chromatography coupled to mass spectrometry were employed to quantify dothiepin in biological fluids, tissues and hair in a death attributed to oral dothiepin (Prothiaden) ingestion. The blood concentration of dothiepin was 5.75 mg/l. Hair analysis clearly indicated a chronic antidepressant exposure, with a dothiepin concentration of 1.89 ng/mg hair. Results are discussed in the light of the existing literature.

Adult↗
PubMed1995

Supercritical fluid extraction of drugs in drug addict hair.

Opiates were extracted from sixteen hair samples of drug addicts using a supercritical fluid extraction method with supercritical carbon dioxide and a modifier solution of methanol-triethylamine-water (2:2:1, v/v). the concentrations, as determined by GC-MS, ranged from 1.22 to 21.73 (mean 7.60 ng/mg), 0.17 to 1.54 (mean 0.69 ng/mg) and 0.15 to 14.009 ng/mg hair (mean 3.78 ng/mg) for codeine, morphine and 6-monoacetylmorphine, respectively. The reproducibility of the total procedure had a relative standard deviation of 13%, 17% and 14% for codeine, morphine and 6-monoacetylmorphine, respectively. But this method, concentrations of 0.3, 0.2 and 0.1 ng/mg hair for codeine, morphine and 6-monoacetylmorphine, respectively, could be detected. Relative extraction recoveries were 61%, 53% and 96% for codeine, morphine and 6-monoacetylmorphine, respectively.

Cannabinoids↗
PubMed1995

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.

3,4-Methylenedioxyamphetamine↗
PubMed1995

Testing human hair for cannabis.

To validate information on cannabis use, we investigated human hair and pubic hair for cannabinoids (THC and THC-COOH) by gas chromatography/mass spectrometry. Samples (100 mg approximately) were decontaminated with methylene chloride, then pulverized and dissolved in 1 ml 1 N NaOH for 10 min at 95 degrees C in the presence of 200 ng of deuterated standards. After cooling, samples were extracted by n-hexane/ethyl acetate after acidification with acetic acid. After derivatization of the dry extract by PFPA/PFP-OH, the drugs were separated on a 30-m capillary column and detected using selected-ion monitoring (m/z 377 and 459 for THC and THC-COOH, respectively). Forty-three hair samples were obtained from fatal heroin overdose cases. Among them, 35% tested positive for cannabinoids. Hair concentrations ranged from 0.26 to 2.17 ng/mg (mean, 0.74 ng/mg) and 0.07 to 0.33 ng/mg (mean, 0.16 ng/mg) of THC and THC-COOH, respectively. As is generally the case for other drugs detected in hair, metabolite concentration was always lower when compared to the parent drug concentration. In public hair, THC concentrations ranged from 0.34 to 3.91 ng/mg (mean, 1.35 ng/mg) and THC-COOH concentrations from 0.07 to 0.83 ng/mg (mean, 0.28 ng/mg). In most cases, the highest cannabinoid concentration was found in pubic hair, suggesting that this sample may be the more suitable for cannabis testing.

Adolescent↗
PubMed1995

Fatal zipeprol intoxication.

A fatality resulting from ingestion of zipeprol is described. Capillary gas chromatography coupled to mass spectrometry was employed to quantify the drug in biological fluids and tissues. The femoral blood concentration of the drug was 2.85 mg/L. Hair analysis clearly indicated chronic drug abuse with a concentration of 7.34 ng/mg. Results are discussed in the light of the existing literature.

Adult↗
PubMed1995

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.

Dextromoramide↗
PubMed1995

Detection of amphetamines in fingernails: an alternative to hair analysis.

After external decontamination, the extraction of amphetamine (AP), 3,4-methylenedioxyamphetamine (MDA) and 3,4-methylenedioxymethamphetamine (MDMA) from hair and fingernails was accomplished via hot alkaline hydrolysis (1 ml 1 N NaOH, 10 min at 95 degrees C) in the presence of deuterated internal standards, followed by a three-step extraction procedure. The target drugs were derivatized by propionylation and analyzed by GC/MS operated in the electronic impact mode. Results indicated that AP, MDA and MDMA were present in both hair and fingernails. Their concentrations, slightly higher in fingernails than in head hair, were 10.2 and 12.0 ng/mg for AP, 8.0 and 9.7 ng/mg for MDA and 53.4 and 60.2 ng/mg for MDMA in head hair and in fingernails, respectively.

Adult↗
PubMed1995

Testing human hair and urine for anhydroecgonine methyl ester, a pyrolysis product of cocaine.

A method using gas chromatography coupled to mass spectrometry for the determination of the cocaine (COC) pyrolysis product, anhydroecgonine methyl ester (AEME), in urine and hair is described. The same procedure allows the simultaneous determination of COC, benzoylecgonine (BZE), ecgonine methyl ester, and cocaethylene. The assay involves acid hydrolysis for hair, deuterated internal standards, a three-step liquid-liquid extraction, and derivatization with N,O-bis(trimethylsilyl) trifluoroacetamide plus 1% trimethylchlorosilane. Detector responses for analytes were linear over the concentration ranges of 0.2-50 ng/mg and 10-2000 ng/mL for hair and urine, respectively. Artifact formation of AEME during the injection was less than 1%. AEME was tested in 65 and 81 cases for hair and urine, respectively, where COC or BZE or both tested positive. Concentrations of AEME ranged from 0.2 to 2.4 ng/mg (n = 7) and from 4 to 226 ng/mL (n = 12) in hair and urine, respectively. Its presence was observed in few cases, clearly indicating that COC smoking is not frequent in France.

Cocaine↗
PubMed1995

Testing human hair for cannabis. II. Identification of THC-COOH by GC-MS-NCI as a unique proof.

To validate information on cannabis use, 11-nor-delta 9-tetrahydrocannabinol-9-carboxylic (THC-COOH) was investigated in human hair. The identification of THC-COOH in hair would document cannabis use more effectively than the detection of the parent drug which might have come from environmental exposure in a smoky atmosphere. Samples (100 mg) were decontaminated with methylene chloride and destroyed by incubation in 1 mL of 1 N sodium hydroxide for 30 min at 95 degrees C in presence of 10 ng of THC-COOH-d3. After cooling, samples were extracted by n-hexane/ethyl acetate after acidification with acetic acid. After derivatization by PFPA-PFP-OH of the dry extract, drugs were separated on a HP1 capillary column, and detected by mass spectrometry (m/z 602) using negative chemical ionization with methane as reagent gas. Among 30 samples obtained from subjects deceased from fatal heroin overdose, 17 tested positive for THC-COOH, in the range 0.02-0.39 ng/mg, with an average of 0.12 ng/mg.

Adult↗