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Y Gaillard

Publications and source records attributed to Y Gaillard.

At least 19 recordsLinked to original sources
PubMed2000

Analysis of corticosteroids in hair by liquid chromatography-electrospray ionization mass spectrometry.

The present study describes a confirmatory method for the quantitative determination in hair of the most common corticosteroids illegaly used as doping agents by athletes. Corticosteroids are extracted from 50 mg of powdered hairs by methanolic extraction follows by a solid-phase extraction on C18 cartridge. After extraction, the dried residue is reconstituted with 50 microl acetonitrile and injected in a liquid chromatograph. Liquid chromatography separation is performed on a reversed-phase C18 column with a binary gradient of formiate buffer pH 3-acetonitrile as mobile phase. Detection is performed with an electrospray ionization mass spectrometer in negative ion and selected-ion monitoring mode. The limits of sensitivity achieved is 0.1 ng/mg in hair. Application to hair sample collected during an antidoping control and comparison to results obtain on urines, collected on the same athletes at the same time, shows the interest and the complementarity of both matrices. Hair analysis could allow the detection of corticosteroids on a large period preceding the control, and the detection of natural corticosteroids administered as pro-drug, like hydrocortisone acetate.

Adrenal Cortex Hormones↗
PubMed2000

Compared interest between hair analysis and urinalysis in doping controls. Results for amphetamines, corticosteroids and anabolic steroids in racing cyclists.

In France during a famous bicycle race, the newspapers documented the degree in which doping seemed to be supervised in some teams by managers and doctors. Use of anabolic steroids and other substances was officially banned in the mid-seventies by sports authorities. This policy has been enforced through urine testing before competition. It is well known, however, that a latency period is all that is necessary to defeat these tests. Nevertheless, hair analysis could be a promising tool when testing for periods that are not accessible to urinalysis any more. We have developed different sensitive methods for testing hair for amphetamines, anabolic steroids and their esters and corticosteroids. For amphetamines, 50 mg of hair were digested with 1 M NaOH, extracted with ethyl acetate, derivatized with TFA and analyzed by gas chromatography positive chemical-ionization mass spectrometry. For corticosteroids, 50 mg of powdered hair were treated with methanol in an ultrasonic bath and subsequently purified using a C18 solid phase extraction column. Analysis was realized by high performance liquid chromatography coupled to electrospray-ionization tandem mass spectrometry. For anabolic steroids and their esters, 100 mg of powdered hair were treated with methanol in an ultrasonic bath for extraction of esters, then alkaline digested with 1 M NaOH for an optimum recovery of other drugs. The two liquid preparations were subsequently extracted with ethyl acetate, pooled, then finally highly purified using a twin solid phase extraction on aminopropyl and silica cartridges. Residue was derivatized with MSTFA prior to injection. Analysis was conducted by gas chromatography coupled to a triple quadrupole mass spectrometer. Thirty cyclists were sampled and tested both in hair and in urine. Amphetamine was detected 10 times in hair (out of 19 analyses) compared to 6 times in urine (out of 30 analyses). Corticosteroids were detected 5 times in hair (methylprednisolone 1 case, triamcinolone acetonide 3 cases and hydrocortisone acetate 1 case) in hair (out of 12 analyses) compared to 12 times (triamcinolone acetonide 10 cases and betamethasone 2 cases) in urine (out of 30 analyses). Anabolic steroids were detected twice (nandrolone 1 case, and testosterone undecanoate 1 case) in hair (out of 25 analyses) compared to none in urine (out of 30 analyses).

Adrenal Cortex Hormones↗
PubMed2000

Fatal aluminum phosphide poisoning.

A 39-year-old man committed suicide by ingestion of aluminum phosphide, a potent mole pesticide, which was available at the victim's workplace. The judicial authority ordered an autopsy, which ruled out any other cause of death. The victim was discovered 10 days after the ingestion of the pesticide. When aluminum phosphide comes into contact with humidity, it releases large quantities of hydrogen phosphine (PH3), a very toxic gas. Macroscopic examination during the autopsy revealed a very important asphyxia syndrome with major visceral congestion. Blood, urine, liver, kidney, adrenal, and heart samples were analyzed. Phosphine gas was absent in the blood and urine but present in the brain (94 mL/g), the liver (24 mL/g), and the kidneys (41 mL/g). High levels of phosphorus were found in the blood (76.3 mg/L) and liver (8.22 mg/g). Aluminum concentrations were very high in the blood (1.54 mg/L), brain (36 microg/g), and liver (75 microg/g) compared to the usual published values. Microscopic examination revealed congestion of all the organs studied and obvious asphyxia lesions in the pulmonary parenchyma. All these results confirmed a diagnosis of poisoning by aluminum phosphide. This report points out that this type of poisoning is rare and that hydrogen phosphine is very toxic. The phosphorus and aluminum concentrations observed and their distribution in the different viscera are discussed in relation to data in the literature.

Adult↗
PubMed1999

Gas chromatographic-tandem mass spectrometric determination of anabolic steroids and their esters in hair. Application in doping control and meat quality control.

We have developed a powerful and simple sensitive method for testing hair for anabolic steroids and their esters. A 100-mg amount of powdered hair was treated with methanol in an ultrasonic bath for extraction of esters, then alkaline digested with 1 M NaOH for an optimum recovery of other drugs. The two liquid preparations were subsequently extracted with ethyl acetate, pooled, then finally highly purified using a twin solid-phase extraction on amino and silica cartridges. The residue was derivatized with N-methyl-N(trimethylsilyl)-trifluoracetamide (MSTFA) prior to injection. Analysis was conducted by gas chromatography coupled to a triple quadrupole mass spectrometer. The generally chosen parent ion was the molecular ion while two daughter ions were selected for each compound with collision energies ranging from -16 to -21 eV. Internal standards were nandrolone d3 for non-esterified drugs and testosterone phenyl propionate for esters. The limits of detection calculated from an analysis of the blanks (n=30) were 0.08 pg/mg for nandrolone, 6.20 pg/mg for boldenone, 0.07 pg/mg for methyl testosterone, 0.15 pg/mg for ethinyl estradiol, 2.10 pg/mg for metandienone, 0.86 pg/mg for testosterone propionate, 0.95 pg/mg for testosterone cypionate, 1.90 pg/mg for nandrolone decanoate, 3.10 pg/mg for testosterone decanoate and 4.80 pg/mg for testosterone undecanoate. Application to doping control has been demonstrated. In a series of 18 sportsmen, two tested positive for anabolic steroids in hair whereas urinalysis was negative for both of them. The first positive case was nandrolone and the second case concerned the identification of testosterone undecanoate. Measured in 10 white males aged between 22 and 31 years, the testosterone concentration was in the range 1.7-9.2 pg/mg (mean=5.0 pg/mg). The method was also applied in meat quality control. Of the 187 analyses realized based upon hair and urine sampling in slaughter houses, 23 were positive for anabolic steroids in hair: one case for boldenone, one case for metandienone, two cases for testosterone propionate, three cases for nandrolone, five cases for testosterone decanoate and 11 cases for methyl testosterone. In the meantime, urinalysis was always negative for these drugs or their metabolites.

Adult↗
PubMed1999

Poisoning by plant material: review of human cases and analytical determination of main toxins by high-performance liquid chromatography-(tandem) mass spectrometry.

The authors have reviewed the main toxic plants responsible for human deaths throughout the world. Forty plants (genera or species) were listed in order to establish an inventory of the active molecules that could be identified, the already published analytical methods and the reported human fatal cases. In a second step, the authors have developed a general method for the detection of various toxins in whole blood by high-performance liquid chromatography coupled to mass spectrometry or tandem mass spectrometry. Sample preparation was realized by liquid-liquid extraction at pH 9.5 for oleandrine, taxol and the alkaloids. These latter compounds were divided into two groups following their chemical properties and could be subsequently purified by acid/base clean up. Cyanogenic compounds and atractyloside were isolated by precipitation of the protein content with acetone and purified for atractyloside by washing with chloroform. Separation of the drugs occurred under reversed-phase conditions on a C18 analytical column 150x2 mm I.D. (5 microm particle size) using two different mobile phases. The first one, formiate buffer 2 mM acidified at pH 3.0, was used for the separation of atractyloside, oleandrine, taxol, the cyanogenic molecules and some alkaloids. The second mobile phase, formiate buffer 10 mM made basic at pH 8.2 was used for the majority of other alkaloids. A gradient elution mode was chosen using acetonitrile or acetonitrile-methanol (50:50, v/v) as the eluting solvent. Detection under positive ionization mode was the mode of choice for all compounds except for atractyloside (negative ions) and for taxol (mixed mode available). Application to real forensic cases has been demonstrated.

Child↗
PubMed1999

Testing hair for pharmaceuticals.

More than hundred pharmaceuticals, drugs of abuse or doping agents have been reported to be detectable in human hair. This article reviews the analysis of 90 drugs and drug metabolites by chromatographic procedures, including the pretreatment steps, the extraction methods, the reported limits of detection and the measured concentrations in real human hair samples. Some progress is observed in the detection of low dose drugs, like fentanyl or flunitrazepam. The general tendency in the last years, to highly sophisticated techniques (GC-MS-NCI, HPLC-MS, GC-MS-MS) illustrates well this constant fight for sensitivity. Some new findings, based on the recent experience of the authors, are also added.

Adult↗
PubMed1998

Gas chromatographic-mass spectrometric quantitation of dextropropoxyphene and norpropoxyphene in hair and whole blood after automated on-line solid-phase extraction. Application in twelve fatalities.

After conversion of norpropoxyphene (NP) to its corresponding amide, dextropropoxyphene (DP) and NP are extracted from 1 ml of blood or 50 mg of powdered hair, on C18 cartridges and eluted using methanol containing 0.5% acetic acid. Automated extraction is conducted on-line with automated device, starting from buffered and centrifuged sample. After extraction, the dried residue is reconstituted with 40 microl of methanol, and then injected in a gas chromatograph at 250 degrees C. Quantitation is carried out by gas chromatography-mass spectrometry in the selected-ion monitoring mode, lidocaine being the internal standard. The method gave relative standard deviations lower than 6.2% in whole blood, and 6.0% in hair for the entire range of calibration from 0.5 to 10 microg/ml in blood and from 1 to 20 ng/mg in hair of both compounds. Limits of detection in blood and hair for DP are, respectively, 0.07 microg/ml and 0.05 ng/mg, whereas the respective limits of detection in whole blood and hair for NP are 0.09 microg/ml and 0.04 ng/mg. The present method was used for one year in our laboratory. Postmortem concentrations of DP in blood ranged from 1.6 to 44.0 microg/ml (mean=9.8microg/ml, n = 12) and are comparable to those found in the literature. Out of 30 hair samples from people who died from heroin overdose, 13 were positive both for DP and NP with concentrations ranging from 0.2 to 27.4 ng/mg (mean 8.7 ng/mg) for DP and 0.3 to 68.9 ng/mg (mean 24.1 ng/mg) for NP.

Adult↗
PubMed1998

Case report of an unusual use of lidocaine during episodes of self mutilation.

We are reporting on a case of polyintoxication by cocaine, lidocaine, methadone, and dextromoramide. This conclusion is supported by the analysis of a strand of hair. We note for the first time the detection of dextromoramide as well as lidocaine and desethyl-lidocaine in hair. Concentrations in hair were: cocaine = 2.4 ng/mg, benzoylecgonine = 0.3 ng/mg, methadone = 10.2 ng/mg, EDDP = 1.5 ng/mg, dextromoramide = 1.6 ng/mg, lidocaine = 115.9 ng/mg and desethyl-lidocaine = 1.6 ng/mg. The victim who was seeking an anesthesia effect without the loss of consciousness ingested cocktails during episodes of self mutilation. The wounds were of two different types and with different morphological locations: long and deep without ablation of tissue, clean lacerations found on the neck, the pectoral region, and the left upper extremity; either round or discoid with deep excavation found on the head (ears, forehead, chin, and lips) and also, on the neck and on the left upper extremity. Near the most recent wounds, needle marks were noticed indicating probable local infiltration of lidocaine.

Adult↗
PubMed1998

Evidence of polydrug use using hair analysis: a fatal case involving heroin, cocaine, cannabis, chloroform, thiopental and ketamine.

A case is presented involving a young woman on several illicit drugs (heroin, cocaine and cannabis) as well as two medications and a solvent used for their anesthetic and narcotic properties: thiopental, ketamine and chloroform. This complex drug use was supported by hair analysis over a 10.5 cm segment of the hair taken at autopsy. The average measured concentrations in hair were: thiopental = 5.3 ng/mg, pentobarbital = 10.0 ng/mg, ketamine = 11.3 ng/mg norketamine = 1.0 ng/mg, diazepam = 1.2 ng/mg, nordiazepam = 0.1 ng/mg, 6-acetylmorphine = 4.4 ng/mg, morphine = 3.4 ng/mg, codeine = 1.2 ng/mg, cocaine = 5.5 ng/mg, benzoylecgonine = 1.5 ng/mg and methylecgonine ester = 1.0 ng/mg. While the ketamine/norketamine ratio is consistent with that already reported on drug detection in hair, the thiopental/pentobarbital ratio seems to be inverted.

Adult↗
PubMed1997

Detection of illegal clenbuterol use in calves using hair analysis. Application in meat quality control.

This study describes a real-life situation involving nine calves, 106 days old, which received oral doses of clenbuterol administered through their milk. Powdered skim milk containing 6.7 mg of clenbuterol was given daily for fifteen days under supervision (i.e. 100 mg per calf for the whole study) to seven calves, and two calves did not receive the drug. Hair samples and urine were taken and subjected to analysis by gas chromatography-mass spectrometry. Hairs were pulverized in a ball mill and 100 mg were incubated in a mildly acidic medium. The sample clean-up procedure involved solid-phase extraction on C18 cartridges. Metoprolol was used as the internal standard for quantitation, after formation of methylboronate derivatives. The calibration curve for clenbuterol in hair was linear in the range 20-5000 pg/mg. The limit of detection of clenbuterol was 16 pg/mg in hair and 0.14 ng/ml in urine. Hair testing was effective after 7-10 days of treatment, and concentrations were in the range of 20 to 4372 pg/mg. Urinalysis can detect clenbuterol for up to two weeks after discontinuation of the drug. Conveniently, this is around the time when the hair samples attain greatest sensitivity. Therefore, the combination of the two matrices appears to be the method of choice for testing for the illegal use of drugs in meat-producing animals.

Administration, Oral↗
PubMed1997

Moclobemide fatalities: report of two cases and analytical determinations by GC-MS and HPLC-PDA after solid-phase extraction.

We have described a rapid and simple solid-phase extraction on C18 cartridges of moclobemide suitable for the analysis of post-mortem whole blood and urine. The methods used for identification were GC-MS and HPLC-PDA. Quantification was performed by the HPLC-PDA technique with detection at 238 nm. The limit of detection was 0.012 microgram/ml in blood. A between-day precision study gave relative standard deviations which were always less than 4.7% over the entire range of calibration (0.2 to 20.0 micrograms/ml). The method was applied in a case of moclobemide overdose due to a deliberate ingestion of 4.5 g of the drug. A second case concerned a polyintoxication including moclobemide as one of the main toxins. The post-mortem whole blood concentrations were 15.5 and 13.8 micrograms/ml respectively. Determination of the drug in other biological specimens is also reported.

Adult↗
PubMed1997

Meprobamate overdosage: a continuing problem. Sensitive GC-MS quantitation after solid phase extraction in 19 fatal cases.

We describe a simple method for the urinary identification and blood quantitation of meprobamate suitable for any toxicological laboratory. After urinary screening using GC-MS technology, quantitation is performed by GC-MS in the selected-ion monitoring mode. Isolation of the drug is achieved by solid phase extraction on a C-18 cartridge. A specific elution is obtained by three volumes of acetone:triethylamine (99:1 v/v). Lidocaine is used as internal standard. RSDs (%) of the within-day and between-day precision studies are always less than 7.2 on the entire range of calibration. Linearity is inspected using an analysis of variance ANOVA. Homogeneity of the variances is tested using Hartley's test. Weighted linear regression is then computed. Limits of detection and quantification are given by an analysis of the blanks. The present method was applied in our laboratory over a period of 1 year. Meprobamate appeared as a drug which still has a significant frequency (5.5%) and is the most frequently involved in fatal pharmaceutical overdoses (15.3%). Post mortem concentrations ranged from 41 to 397 mg/l (mean = 182) and are compared to those of the literature.

Analysis of Variance↗
PubMed1997

Simultaneous solid-phase extraction on C18 cartridges of opiates and cocainics for an improved quantitation in human hair by GC-MS: one year of forensic applications.

We have developed a new solid-phase extraction (SPE) on C18 cartridges which allows a very simple protocol of manipulation and a single elution of opiates and cocainics from human hair samples. The method involved decontamination in a phosphate buffer and dichloromethane, pulverization in a ball mill, addition of deuterated internal standards, heated acid hydrolysis and SPE. Quantitation utilized gas chromatography and mass spectrometry. Between days precise study gave relative standard deviations always inferior to 8.9% for each compound at 4 ng/mg (except methylecgonine ester = 15.7%). Accuracy was tested using a t-statistic versus a reference material from the NIST. Limits of detection were calculated from an analysis of the blanks which contained between 0.12 and 0.28 ng/mg for each drug. The method was applied in forensic cases for 1 year of toxicological activity. Among the 108 analyses performed, 30 were positive for cocaine and 33 for opiates. Concentrations were in the range 0.9-242.0 ng/mg (cocaine), 0.3-71.3 ng/mg (benzoylecgonine), 0.0-9.8 ng/mg (methylecgonine ester), 0.0-2.9 ng/mg (cocaethylene), 0.1-11.5 ng/mg (codeine), 0.4-44.6 ng/mg (morphine) and 0.7-131.2 ng/mg (6-acetylmorphine). Ratios of the metabolites to parent drugs were proposed to avoid risk of external contamination.

Cocaine↗
PubMed1997

Use of high-performance liquid chromatography with photodiode-array UV detection for the creation of a 600-compound library. Application to forensic toxicology.

A high-performance liquid chromatographic method is described with photodiode array detection for systematic toxicological analysis in human blood and urine. After a single step liquid-liquid extraction using Toxi-Tube A, drugs are analyzed with a multi step gradient (phosphate pH 3.8-acetonitrile) on a Symmetry C8 5-microns column (250 mm x 4.6 mm I.D.) (Waters), operated at 30 degrees C. The flow-rate is varied during the run from 1 ml/min to 1.5 ml/min. Full UV spectra are recorded on-line during the 28 min chromatographic run. Enhanced performances for drug detection are obtained with this method due to (a) reduction of peak-tailing for basic drugs, (b) lower identification limits, (c) more stable retention times and (d) larger number of referenced drugs (684 spectrum registered). Application of real samples has been demonstrated.

Adult↗
PubMed1997

Screening and identification of drugs in human hair by high-performance liquid chromatography-photodiode-array UV detection and gas chromatography-mass spectrometry after solid-phase extraction. A powerful tool in forensic medicine.

A method is described to screen for a wide range of pharmaceuticals in human hair. 75 mg of powdered hair are incubated (12 h at +56 degrees C) in 2 ml of distilled water (acidic compounds) or 0.1 M hydrochloric acid (neutral and basic compounds). A twin solid-phase extraction on C18 cartridges is used for the sample clean-up procedure. Acidic drugs are fixed at pH 2 and eluted with 1% ammoniacal methanol while neutral and basic drugs are retained on the column at pH 8.6 and eluted with methanol containing 0.5% acetic acid. The internal standard (I.S.) for the acidic extraction was bupivacaine while the I.S. for the basic extraction was prazepam. The separation of the drugs was performed using both the liquid and the gas chromatographic techniques whereas identification was achieved using photodiode array and mass spectrometric detection, respectively. The liquid chromatographic system gives an elution of the drugs following a multi step gradient from a Symmetry C8 (Waters) 5 microns column (250 x 4.6 mm I.D.) at +30 degrees C with acetonitrile-phosphate buffer (pH 3.8). Identification is achieved using the reference data (retention times and spectra) of 675 pharmaceuticals, toxicants and drugs of abuse stored in a personal library. The present method has been applied during 6 months in our laboratory. By establishing a victim's drug use history, it is a very powerful tool in forensic medicine. We illustrate the method with some real cases of police crime investigation.

Adult↗
PubMed1997

Concordance between self-reported drug use and findings in hair about cocaine and heroin.

We have presented the results concerning 135 judicial expert opinion over a 3-year period. We have compared the measured levels in hair of 6-acetylmorphine (6-AM) and of cocaine with the habitual use declared by the consumers. This allows us to propose three levels (low, medium, high) of consumption in relation to the level of the 6-AM marker found in hair for the consumption of heroin, and the level of cocaine as a marker for the cocaine intake.

Biomarkers↗
PubMed1996

Coin-operated dry cleaning machines may be responsible for acute tetrachloroethylene poisoning: report of 26 cases including one death.

BACKGROUND: Incorrect operations by customers are not uncommon in coin-operated dry cleaning establishments; dry cleaning machines may also be poorly maintained. This may result in retention of large amounts of the cleaning solvent in dry cleaned items. CASE REPORT: A 2-year-old boy was found dead in his bed, with a strong odor of solvent in the room. Toxicological analysis demonstrated tetrachloroethylene poisoning. The solvent had been retained in the double curtains of the bedroom which had been dry cleaned in a coin-operated establishment the same day. A retrospective study at the Paris Poison Center revealed 25 additional cases, all with a favorable outcome. Analysis of the circumstances of these accidents showed that the main causes of tetrachloroethylene retention in clothes are overloading of the machine and dry cleaning of bulky items. However, failure of the dry cleaning machine may also be involved. CONCLUSIONS: To immediately reduce the health risks, consumers were informed both via the mass media and by warnings in coin-operated dry cleaning shops. A second batch of preventive measures is in preparation including modifications of the machines to limit solvent exposure and a specific regulation concerning their inspection and maintenance.

Adult↗