Quantitative determination of taxine B in body fluids by LC-MS-MS.

A new specific and sensitive LC-MS-MS method for the detection of taxine B and isotaxine B, the main toxic pseudo-alkaloids from yew (Taxus sp.), in biological samples (blood, urine, gastric content) was developed. Biological samples were prepared for LC-MS-MS by means of solid-phase extraction (SPE) procedure and yielded a recovery of 86%. Chromatographic separation was achieved using an RP(18) column. Detection of taxine B and isotaxine B was performed using multiple reaction monitoring with m/z 584.2 as precursor ion, i.e. [M+H](+), of both isomers and m/z 194.3 and m/z 107.1 as product ions after collision-induced dissociation. Docetaxel was applied as internal standard. The method was fully validated for the analysis of blood samples. Linearity was proven in the range from 0.1-500 ng/g. The limit of detection and the limit of quantitation are 0.4 and 2 ng/g, respectively. The method was applied to the determination of taxine B and isotaxine B in four fatal cases (two humans, two horses) with suspected yew intoxication. Blood levels were 105, 168, 174 and 212 ng/g.

[Criminal and suicidal death with bolt gunshot weapons. An experimental and case contribution]. / Kriminelle und suizidale Tötungen mit Bolzenschussgeräten. Ein experimenteller und kasuistischer Beitrag.

Authors report on two cases of homicide and another case of suicide, all committed with captive-bolt livestock-stunners. The investigation of skull caps revealed roundish holes at the entry sites which were beveled-out in a paraboloid-like manner on the inner aspect. These defects were reproducible in test shots with various strengths of ammunition and different materials as targets.

Clinical and morphological aspects of death due to liquid nitrogen.

A 24-year-old student died while filling flasks with liquid nitrogen. The arms, legs and back were frozen and the face, ears and neck showed a dark red and livid colour with horizontal lines of demarcation. In the electrocardiogram, the heart showed asystolia followed by wide ventricular complexes. The patient was intubated orally as the situs of the larynx and pharynx showed no pathology findings. Cardiopulmonary resuscitation was carried out and terminated after 90 min. Unfortunately, the body temperature was not measured. The gas analysis of venous blood showed metabolic acidosis and oxygen deficiency. The student had worked alone with nitrogen, without opening the windows and without a working ventilation system. While filling the third flask he lost consciousness. As nitrogen does not cause characteristic prodromal signs he laid on the floor and was unable to help himself. The liquid nitrogen which was still escaping spread over the floor and vaporized. The student died from asphyxia due to oxygen deficiency in an atmosphere of nitrogen.

[Heavy metal incorporation as an unusual self-injury]. / Schwermetall-Inkorporation als ungewöhnliche Selbst(be)schädigung.

A 19-year-old man was admitted to hospital because of uncharacteristic neurologic symptoms. During the first examination morphologic alterations due to an injection of mercury into the left arm and the left side of the trunk were found. The dose and the manner of application were doubtful and suspected to be a case of self-infliction. The man informed the police only 7 months later because his relatives had finally persuaded him to do so. The description of the infliction by unknown perpetrators was full of contradictions. Initially the patient gave only an indistinct description. But later on, the number of details increased. At the same time there was a change in the characteristics of the perpetrator(s). Other differences existed concerning a loss of consciousness which should have been caused by a single stroke on an arm. Furthermore, the patient told about a swelling as big as an egg, provoked by an injection of liquid mercury. It could be shown by experiments that mercury can be injected into soft-tissue very simply and that it spreaded widely. Arguments for a self-injection were e.g. the technical possibility, the topography of the injection marks, and an easy handling of the syringe. A psychiatric examination furthermore revealed, that the patient had had periods of restriction of thinking, sometimes combined with a lack of appreciation.

[Falsification of breath alcohol concentration measurement. An experimental and case report]. / Zur Verfälschung der Messung der Atemalkoholkonzentration. Ein experimenteller und kasuistischer Beitrag.

As a rule, in our comparison of breath alcohol and blood alcohol concentration levels both readings were in agreement. Nevertheless, we repeatedly observed readings showing significant differences for which there was no apparent explanation. In two cases where discrepancies were extreme (breath alcohol concentration greater than 2.0%; blood alcohol concentration, 0.0%) we discovered that the cause was sniffing. The effects of various pharmaceutical drugs were tested. Experimentally the inhalation of liquid gas resulted in ostensible breath alcohol concentration levels of more than 2%. These experiments were reproducible. Consequences for the exployment of alcohol breath testing devices are discussed.

[FTIR-microspectrophotometry for high resolution and highly sensitive detection of the carboxyhemoglobin complex]. / FTIR-Mikrospektrophotometrie zur hochauflösenden und hochempfindlichen Detektion des Carboxyhämoglobin-Komplexes.

Our recently developed method for rapid quantitative evaluation of carboxyhemoglobin in liquid as well as in dried blood samples has been considerably improved by the incorporation of an infrared microscope. Besides the characteristic bands at V = 1953 (cm-1) in liquid and V = 1968 (cm-1) in dry blood we found, upon addition of D2O, a dislocation of the bands at V = 1949 (cm-1). This reversible dislocation still permits a reliable identification of the COHb complex at the extremes of the capacity range of the measuring unit. Thus identification of the COHb complex was successful even in isolated erythrocytes. By means of this improved technique reliable quantitative evaluation may be carried out in a concentration range of between 2% and 0.05% whereas semiquantitative evaluation was possible at concentration down to 0.01%, allowing for instance the evaluation of the effects of a single inhalation of cigarette smoke. The positive identification of endogenous COHb fractions as well as of exogenous agents (smoking, environmental factors) which this method permits is prerequisite for a dependable interpretation of forensic-toxicologically relevant COHb findings.

Acetonitrile serum concentrations and cyanide blood levels in a case of suicidal oral acetonitrile ingestion.

Acute acetonitrile toxicity is mainly dependent on the release of cyanide via hepatic metabolism. Although evaluated in animals, few data are available concerning the toxicokinetic parameters of acetonitrile and acetonitrile-liberated cyanide in human. This paper reports a case of suicidal oral acetonitrile ingestion of about 5 mL without severe symptoms of intoxication in a previously healthy adult male with a body weight of 60 kg. Acetonitrile serum concentrations as well as cyanide blood levels were determined over the whole hospitalization. The elimination half-lives calculated from these data were 32 h for acetonitrile and 15 h for cyanide. After sodium thiosulfate bolus application, the cyanide blood level rapidly decreased to 10% of the initial value, indicating that sodium thiosulfate sufficiently detoxifies acetonitrile-liberated cyanide. Since cyanide levels again increased to maximal values about 4.5 h after sodium thiosulfate application, continued thiosulfate therapy is required as predicted by the long elimination half-lives of acetonitrile and acetonitrile-liberated cyanide. Determination of cyanide and acetonitrile concentrations is recommended for the estimation of optimal individual sodium thiosulfate dosage.

[Chloroquine as a poison in murder. Report of fatalities after criminal or suicidal chloroquine administration]. / Chloroquin als Mordgift. Mitteilung über Todesfälle nach krimineller und suizidaler Chloroquinbeibringung.

Presented is a case of murder by means of chloroquine, committed on a 36-year-old male. The wife of the deceased had confessed to have secretely administered chloroquine-containing tablets to her husband. She was lawfully sentenced to life-imprisonment. The toxicological findings of this case are compared to the results of two chloroquine suicide cases and discussed in the context of the referring literature. An additional case where chloroquine intoxication was doubtful is introduced because of the unusual circumstances under which it occurred.

Chronic enteral poisoning caused by potassium permanganate: a case report.

To our knowledge, this is the first case report of a multiple, low dosage ingestion of manganese. A 66-year-old male patient is presented, who ingested 125 ml of a 8% solution of potassium permanganate (10 g) within 4 weeks. As early as 2 weeks after the beginning of poisoning, psychological alterations were noted. Neurological examination revealed disturbances of many subsystems of the CNS. Visually evoked potentials showed prolongation of the P2-latency, not reported in earlier publications. Levels for manganese were elevated in peripheral blood as well as in hair samples. Treatment with calcium trisodium pentetate decreased serum levels and increased urine excretion of manganese. Nine months after poisoning, the first signs of progressive Parkinson disease became evident. The time-course of neurological symptoms seems to depend on a critical dose of manganese.

[Quantity of weapon oils at the target as a function of shooting sequence and firing distance]. / Die Waffenölmenge am Ziel als Funktion der Schussreihenfolge und der Schussentfernung.

Five widely used gun oils were tested to see if they could be identified by gas chromatography. All oils in the test produced characteristic gas chromatograms and the test was highly sensitive in tracing the oils. Seven different weapons and various types of ammunition were used to perform firing tests involving an oil sold under the brand name of "Gun pro." The weapons were oiled and wiped dry and subsequently discharged at a cotton cloth target. Series of shots were fired from a maximal distance of 3 m, and the weapon was not cleaned between shots. Grease marks and powder-burn traces were extracted separately and the extracts, after adding an internal standard, were investigated by means of gas chromatography (gas chromatography unit by Perkin and Elmer). The largest quantities of oil were transmitted by indoor ammunition fired from a small-bore rifle. At a firing range of 20 cm, a decrease in the oil quantity could be observed up to the fourth discharge. When the firing range was varied there was a decrease in the oil quantity up to a distance of 80 cm. The first and the second discharge could be distinguished up to a firing range of 60 cm. With increasing force of the projectile and a decrease in the interior length of the gun barrel, the quantity of oil conveyed to the target also decreased. Additionally, the identifiability of the oil was investigated after firing at several layers of cloth and after storage of the samples (no losses occurred after a 1-month storage period).(ABSTRACT TRUNCATED AT 250 WORDS)

[Atypical bullet entry injuries. A case report and experimental contribution]. / Untypische Einschussverletzungen. Ein kasuistischer und experimenteller Beitrag.

In order to elucidate the contradictory findings in cases of suicide or homicide with firearms, firing tests were performed with various weapons shot at textile samples, block gelatine, animal and human skin, and pigs' heads. Ricochets were produced at different angles of incidence and bullets were shot through various materials introduced between the target and muzzle. The morphology and emission spectrum analyses of the entry holes were investigated, and the projectiles were collected and inspected. The morphological and chemical alterations observed at the entry holes were classified and discussed.

[Reproduction of atypical bullet exit wounds]. / Zur Reproduktion atypischer Ausschusswunden.

Contradictory findings from experiments designed for the reconstruction of the circumstances in crimes committed with firearms induced us to systematically investigate the conditions leading to the occurrence of non-typical bullet exit wounds. For this purpose, skin samples and pig heads were fired at with different types of small arms and, on the exit side, the skin was brought into contact with various materials. The bullet exits were investigated morphologically and by means of emission spectrum analysis. The results from these investigations are classified and discussed.

[A new method for the determination of carboxyhemoglobin in fluid and dried blood using Fourier transformation infrared spectrometry]. / Eine neue Methode zur Carboxyhämoglobinbestimmung in flüssigem und getrocknetem Blut mittels Fourier-Transform-Infrarot-Spektrometrie (FTIR).

A new technique is presented for the fast quantitative determination of carboxy-hemoglobin (CoHb) in liquid blood with the aid of Fourier transformation infrared spectrometry. The bands at v = 1953 and 1969 (cm-1), which are characteristic for the CoHb complex, were measured without the blood being prepared. In liquid samples the band at 1953 cm-1 is prominent; in dry samples, however, it appears. In moist samples both bands--each to be coordinated with a different CoHb conformer--are observed at about the same intensity. Even with dried blood spots of less than 0.1 mg, quantitative determination of CoHb at v = 1969 (cm-1) is possible. Systematic investigations of the thermic stability of the CoHb complex were performed. The typical interference phenomena associated with UV spectrometry were not observed when the above-described method was employed nor are they to be expected. Even under extreme measuring conditions, as for example when measuring transmission through lab-coat material, different CoHb contents could be determined in traces of dried blood.

[Deferoxamine in hemosiderosis. Fecal iron excretion during continuous subcutaneous infusion]. / Deferoxamin bei Hämosiderose. Fäkale Eisenausscheidung während kontinuierlicher subkutaner Infusionen.

Faecal iron excretion during continuous subcutaneous deferoxamine infusion was measured by flameless atom-absorption spectral photometry in 21 patients with homozygous ss-thalassaemia and one patient with Blackfan-Diamond anaemia. Taking into account faecal and urinary iron excretion, more iron was eliminated than was taken up during transfusion and by intestinal absorption. Urine contained 37.9%, faeces 62.1% of the amount of iron eliminated.

[Nature of the black zones in hair following ingestion of thallium]. / Zur Natur der Schwärzungszonen in Haaren nach Thalliumaufnahme.

A total of 510 hairs with Widy's zones from 6 cases of poisoning were microscopically studied, both with light from above and from below. In every instance when the light came from below the zones appeared lighter in colour when pressure was applied. This lighting-up in color was reversible. This effect is incompatible with the opinion, still prevalent today, that the zones may be explained by hyperpigmentation. Quite frequently the zones became lighter during a prolonged exposure to water while simultaneously gas bubbles developed. However, even after extensive exposure to thioglycolic acid the zones did not disappear entirely in all cases. We explain these phenomena with the total reflection of the light at numerous bordering surface of substances with differing indices of fraction. We measured the thallium concentration in the urine and in the hair during the time interval between two thallium poisonings with the result that in those parts of the hair which had grown during a period when no thallium level was measured in the urine we found discernibly to strongly increased thallium concentrations. The results of our study indicate that, considering the most recent knowledge, proof of multiple thallium poisoning ought not to be attempted by means of fractional chemical investigation of the hair alone.

[Perforation of the large intestine caused by compressed air. Experimental studies reconstructing compressed air insufflation]. / Dickdarmperforation durch Pressluft. Experimentelle Untersuchungen zur Rekonstruktion einer Druckluftinsufflation.

A foreign worker died after a compressed air injury. The insufflation of high pressure air into the anus caused multiple ruptures in the part anterior of the dilated sigmoid and colon descending. For the reconstruction of the case it was necessary to know the minimum distance between the nozzle and the gluteal region. Experimental work has shown that clothing does offer protection against the high pressure air and colon perforations can only be expected if there is a small distance between the jet of the compressed air and the anal region.

[Determination of lead in hydride form in bone biopsies of patients with long past lead poisoning]. / Der Nachweis von Blei als Hydrid in Knochenbiopsieproben von Patienten mit lange zurückliegenden Bleivergiftungen.

Disturbances in the determination of lead by means of flameless atomic absorption by highly pure CaCl2-solutions were demonstrated. To avoid such disturbances a new method for estimation of lead in bone specimens is introduced. Lead is separated in hydride form by adding NaBH4 to the specimens in an acid solution containing tartaric acid and sodium dichromate in a so called metal-hydride-system and then identified by atomic absorption spectrophotometry. For higher concentrations or for mass spectrometric determination of the lead isotope proportions the lead hydride may also be frozen. The hydride method has been used with the estimation of lead in biopsy specimens from the iliac crests of 14 patients who suffered from nephropathies of unknown origin. In addition flameless AAS was employed and the results were controlled. The lead contents in bone specimens from 13 patients with a long history of occupational exposure to lead varied between 126 mumol/kg (26 micrograms/g) and 1,97 mmol/kg (410 micrograms/g) of dried substance. In five control specimens the corresponding values ranged from 19 mumol/kg (4 micrograms/g) to 87 mumol/kg (18 micrograms/g). These findings suggest that nephropathy results from body burden of lead. Additionally hair specimens and nail clippings from several of the above patients were analysed. Control analyses were carried out. The question of lead release from deposits in bone and the connections between nephropathy and exposure to lead are discussed.