Gas chromatographic determination of cresols in the biological fluids of a non-fatal case of cresol intoxication

A simple and rapid method for analysis of free and conjugated cresols in biological fluids was developed. Prior to and following freeing of the conjugated cresols by acid hydrolysis in a sealed ampoule, free cresols were extracted by Extrelut column extraction, determined by gas chromatography, and confirmed by gas chromatography-mass spectrometry. In a non-fatal case of cresol intoxication a 46-year-old male had ingested about 100 ml of a saponated cresol soap solution. The concentrations of xylenol (2,4- and/or 2,5-dimethylphenol) and p- and m-cresol in the serum sample collected on admission were 15.8 micrograms/g, 43.3 micrograms/g and 73.8 micrograms/g, respectively. The total cresol concentration of 117 micrograms/g in the serum is within the range of fatal concentrations, and it is suspected therefore that the patient's recovery was due to adequate therapy alone.     

A gas chromatographic method for determining acetaldehyde in cadaver blood

Gas-chromatographic method of acetaldehyde detection in blood of subjects who died of alcoholic intoxication is suggested. Method is simple, does not require additional expenses, can be readily used in medicolegal practice and in difficult cases it may help the expert to make an objective conclusion on the cause of death.     

体液中微量士的宁的富集及同时检测

目的将分子印迹技术运用到法医毒物分析中,建立一种全新的测定体液中微量士的宁的方法。方法运用分子印迹原位聚合技术,在色谱柱中一步合成了对士的宁具有专属识别能力的分子印迹聚合物,以此聚合物为介质,装填一厘米的小柱,建立体液中微量士的宁的富集及同时检测方法。结果以士的宁分子印迹聚合物作为尿液和血浆中微量士的宁的富集和检测介质,方法的检出限为4.9ng,样品回收率均大于92%,相对标准偏差小于6.59%,工作曲线的线性相关系数分别为0.9991和0.9966。运用此方法对中毒家兔血浆和尿液中的士的宁进行了测定。结论建立的新方法可以实现对士的宁专属的、灵敏的检测,适合于法医学毒物分析运用。     

The gas chromatographic determination of carbophos in cadaveric material

The authors developed a method of malathion insecticide determination in the cadaveric material (blood and wall of the stomach) including extraction of 5 ml of blood (5 g of fragmented tissue of stomach wall) by hexan; preparative chromatographic purification of extract on silicagel layer L 5/40 mkm in hexan-diethyl ether system 10:2; Gas-liquid chromatographic investigation on column with 5% SE-30 and 5% XE-60 (Chromatograph "Colour-106" with thermionic detector). This method makes it possible to detect 72-76% of malathion added.     

A gas chromatographic method for detecting nitrites in the blood and stomach contents

Ethyl nitrite method is proposed as the tentative test for nitrites in studies of the blood and gastric contents. The sensitivity of the method in "pure" solutions is 17 micrograms/sample. The method is specific and its sensitivity is not inferior to routine chemical analyses of biological materials for nitrites.     

A gas chromatographic analysis of phosphine in biological material in a case of suicide

In a suicide committed using aluminium phosphide (AlP) the liberated toxic phosphine gas was detected in post-mortem specimens using a headspace gas chromatographic procedure with a nitrogen-phosphorous detector (HS-GC/NPD). At autopsy a direct sampling into airtight headspace vials for a later analysis is recommended. AlP has to be considered a potent pesticide and its use and availability should be restricted as much as possible.     

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.     

The chromatographic analysis of phencyclidine, its metabolites and analogs in biological fluids

Reviews data on analysis of narcotic phencyclidine and its main metabolites and analogs. Pharmacological and toxic characteristics of phencyclidine, conditions of its isolation from biological objects and its detection and measurement by thin layer and gas chromatography and by chromatographic mass-spectrometry are described. Analysis of phencyclidine metabolites is discussed and a scheme of its metabolism is presented. Statistical characteristics of methods of quantitative analysis of phencyclidine in biological objects are presented.     

A rapid gas chromatographic method for the fingerprinting of illicit cocaine samples.

A gas chromatographic (GC) fingerprint method, based on the presence or absence of six congeners, was developed for illicit cocaine samples. The fingerprint utilizes the relative abundances of these congeners towards each other, disregarding cocaine as the main constituent, and can be expressed numerically or graphically in the form of pictograms for rapid visual comparison. The method can be applied directly to a solution of the sample in chloroform, without previous workup procedures. More than 70 unrelated samples were analyzed and a great variation was observed in the parameter composition. On the other hand, a remarkable similarity could be seen between related samples. The GC fingerprint method may be considered an important contribution for sample comparison, as is exemplified by a subdivision of the analyzed samples in different categories, based on the number and types of congeners found.     

生物材料中二氯苯醚菊酯的反相高效液相色谱分析方法研究

目的为了解决二氯苯醚菊酯中毒检验的问题及进一步开展研究工作，建立多种生物材料中二氯苯醚菊酯高效液相色谱分析方法。方法选用shim—pack，CLC—ODS（5μm）作色谱柱，甲醇：水：冰醋酸（90：10：1）为流动相，检测波长为274mm。用空白添加试验系统地考察提取，净化方法及高效液相色谱分析条件。用日本大耳兔进行急性染毒，取材对所建方法进行验证。结果采用所建方法，空白组织添加回收率在0．2～20μg／g的范围内均大于85％；工作曲线线性良好（r＝0．9998）；以信噪比≥3计，最低检测限为10ng／g组织；方法重现性良好（CV＜4．5％，n=3）；染毒兔各组织中的内源性杂质均不干扰二氯苯醚菊酯的检测。结论所建方法适用于检测多种生物材料中的二氯苯醚菊酯，方法灵敏、准确，可望用于二氯苯醚菊酯的中毒检验、代谢动力学及分析毒理学的研究。     

生物材料中二氯苯醚菊酯的反相高效液相色谱分析方法研究

目的 为了解决二氯醛醚菊酯中毒检验的问题及进一步开展研究工作，建立多种生物材料中二氯苯醚菊酯高效液相色谱分析方法。方法 选用ｓｈｉｍ－ｐａｃｋ，ＣＬＣ－ＯＤＳ（５μｍ）作色谱柱，甲醇：水：冰醋酸（９０：１０：１）为流动相，检测波长为２７４ｎｍ。用空白添加试验系统地考察提取，净化方法及高效液相色谱分析条件。用日本大耳兔进行急性染毒，取材对所建方法进行验证。结果 采用所建方法，空白组织添加回收率在０．     

Brain acetaldehyde and ethanol: method of determination and diagnostic significance in ethanol poisoning

The content of ethanol and acetaldehyde in the limbic cortex and reticular formation of the brain was measured by gas-liquid chromatography in lethal ethanol poisoning. The content of acetaldehyde was significantly increased in the gyrus cinguli of the brain. Lethal poisonings occurred during any stage of ethanol intoxication. The data characterizing individual ethanol tolerance were obtained, which can be used for differential diagnosis of ethanol poisoning in practical forensic medicine.     

Research of the extraction method of morphine from biological fluids

A solid-phase extraction method of morphine from urine and blood has introduced. The effect of 5 SPE columns, 3 eluents and pH on morphine recovery has been investigated systematically. Derivative GC was used as a method of detection. The result showed that the column and the eluent of such as GDX-301, GDX-403 and C18 chloroform:isopropanol (9:1) had good behaviors to extraction of morphine. When GDX-301 was used as a sorbent, the recovery of morphine from urine was above 90% at pH 9, then went down with the increase of pH. While the recovery from blood was growing with the increase of pH, which reached above 90% in strong alkaline. The extraction method is simple, inexpensive, efficient and reproducible, which provides an effective and practical method to extract morphine and similar illicit drugs from biological fluids.     

Simple determination of carboxyhemoglobin by double wavelength spectrophotometry of absorbance difference and the comparison with gas chromatographic method

This paper describes the spectrophotometric determination of carboxyhemoglobin (CO-Hb) in blood on the basis of double wavelength spectrophotometry of absorbance difference. Absorbance measurements are made in the 500–600 nm region at a blood dilution of 100–200-fold. Blood is diluted with a solution containing Na₂S₂O₄ to provide two components of CO-Hb and deoxyhemoglobin (deoxy-Hb). Absorbance difference at the two wavelengths at which deoxy-Hb has the same absorbance reflects only the CO-Hb component because the opposite component is nulled out of the mixture. After measurement of the absorbance difference, the measuring solution is saturated with CO gas to make all Hb derivative CO-Hb and remeasured at the same wavelengths. The percent of CO-Hb is considered the absorbance difference ratio. Results obtained by the present method was in satisfactory agreement with gas chromatographic data in blood not containing methemoglobin (Met-Hb). Comparative experiments using the gas chromatographic method and the present method were performed with samples containing Met-Hb. However, while there is a deficiency in the gas chromatographic method when the samples contain Met-Hb, the results of the present method were in close agreement with theoretical values when samples are mixed with CO-Hb, O₂-Hb and Met-Hb. Advantages of this method are that it is simple and accurate, standard curve or equation for calculation and accurate dilution are not necessary.