高效液相色谱法测定人血清中安眠酮及其苯甲基羟化代谢物的浓度

本文建立了用反相高效液相色谱法(RP-HPLC)测定人血清中安眠酮及其苯甲基羟化代谢物-2-甲基-3[2-(羟甲基)-苯基]-4(3H)喹唑酮(Ⅰ)的浓度。安眠酮浓度在1-35μg/ml范围内呈直线相关(相关系数r=0.9980;回归方程y=0.06324x—0.1029),方法回收率平均为102.08±9.987(SD)％(n=5),检出限为1ng。其代谢物Ⅰ按原型安眠酮的线性浓度测定其相对量。本法为测定中毒者体内安眠酮及其代谢物Ⅰ的血浓度提供可行的手段。     

安眠酮及2'-羟甲基安眠酮的毛细柱GC/MS测定

作者在 Finnigan Mat 1020 GC/MS 仪上,应用 SE-54熔融硅毛细柱,建立了生物试样中安眠酮、2'-羟甲基安眠酮的分析方法。动物中毒实验表明,此法实用,不仅能检出安眠酮,而且还可检出存在的代谢物;在实际应用中,具有快速、灵敏、准确等特点。检测限为15ng,并已用于刑事案件的鉴定工作中。     

尿样中安眠酮代谢物的分析

安眠酮是一种作用时间快、半衰期长的低毒性镇静催眠药物,长期服用有一定的成瘾性,目前国际上已将此药列为滥用药品,控制其生产和使用。由于安眠酮的代谢周期长,在体内容易积累,其代谢物     

尸体脏器中几种镇静药物气相色谱/质谱测定的研究

本文应用气相色谱/质谱(GC/MS)技术,研究了尸体脏器中五种巴比妥酸盐、导眠能、苯妥英的定性和定量分析方法。应用SE-54毛细柱找到了良好分离条件。以安眠酮作内标,建立了定量分析程序。应用这个方法,可在1小时内完成定性分析,检测限为5ng;定量分析的准确度和精密度均为±10％。     

血中安眠酮的硅藻土提取紫外导数光谱测定法

固相革取是一种新的分离方法，和传统的液液革取法相比，具有革取率高、操作简单、省溶剂、避免乳化等优点。固相革取法按所用的固棺材料可分为亲脂性材料（如烷基键合相硅胶。大孔树脂）固相苹取和亲水性材料（如硅藻土、硅胶）固相革取两种。对于亲脂性材料革取，国内已有较多的研究，而亲水性材料固柏章取，国内尚未见报道。笔者建立了血中安眠酮以硅藻土为因相材料进行提取、用紫外导数光谱进行测定的方法。此法操作较用亲脂性因相材料车取更为简单、快速，回收率也高。实验方法一、主要仪器。试剂、材料日本岛津Uv－250型紫外可见分光…     

广东精神类毒品犯罪趋势

近年来,中国毒品形势发生了新的变化,制贩“冰”毒和非法买卖、走私易制毒化学品等新型毒品犯罪迅速发展蔓延。特别是受港澳台境外黑社会毒品犯罪方式的影响与渗透, 在广东、福建等地,毒品犯罪分子不仅制贩海洛因、可卡因等常规毒品,而且开始制造、贩卖“冰”毒。以广东省为例, 从1991年至2004年4月,广东省公安机关共侦破各类制贩精神类毒品案件218宗(其中制贩“冰”毒案件94宗、制贩“摇头丸”案件124宗),共缴获“冰”毒约47吨、“摇头丸”388余万粒、氯胺酮1605千克、安眠酮近3300千克(氯胺酮和安眠酮截止2003年6月),摧毁制毒工厂、窝点89个。     

应用HPLC对常见药物的筛选分析

作者采用高效液相色谱(HPLC),对常见的酸性、碱性及某些中性提取药物约50多种进行了分离,以安眠酮作内标,对常见药物进行筛分。按其对内标物的比保留时间(RRT)值可提供是那种或属那类药物,以再进一步分析或以GC/MS作确证分析。此法具有缩小分析范围,快速定性、定量的实用性。     

HP5971A质量选择检测器对滥用药物分析的临床评价

<正> 我们对用于实验室分析的一种新型的5971A质量选择检测器(MSD)进行临床评价。这种新型检测器宽7英时,实验室人员在三个月的时间里对大约120名病人的尿样中的十种常见滥用药物进行了分析,以证实HP5971A MSD的临床性能。控制分析证明了5971A MSD的准确度和精密度。所分析的尿样分别含有Ptncyclicline,速可眠,安眠酮。每种药物分     

混合碱性药物中毒检验一例

<正> 一、案情摘要某男,1987年5月12日在家中突然死亡。死者之妻,于5月8～10日将安定250片、利眠宁100片、安眠酮18片研成粉末分六次掺入麦乳精、牛奶、糖水中给丈夫服下。10日晚,见夫未死,又向其静脉注射空气,并用浴巾、纱巾、棉被等物捂夫的口和鼻,但仍未将其捂死。     

美国庸医知多少

在美国加州圣迭戈市,一外科整形医生欲从病人的臀部取出癌瘤,但他却错砍下一块厚厚的健康骨组织,造成病人臀部严重骨折,而体内的癌瘤却完好无损。 在佛罗里达州奥兰多市,一位皮肤病“专家”曾34次被指控渎职,但依然逍遥行医。他的行医执照被吊销时,原因并非是不胜任工作,而是向便衣警官出售了1000片安眠酮。 象这样的案例不胜枚举。无照营业或虽有执照但毫不称职的庸医正严重危害着美国公民的身体健康,其数量之多,令人惊恐。 据美国国家医学联合委员会执行副总裁伽鲁西博士透露,美国无照行医者占医生总数的5％,大约有25,000人。一位名叫乔治·阿萨克的“医生”唯一能证明他的医生身份的是在纽约的一台录音电话机。有指证说,去年     

The human distribution of some barbiturate sedatives in combination with miscellaneous CNS-active drugs

This paper presents 14 cases in which the distribution of barbiturates and the hydroxylated metabolites in combination with miscellaneous CNS-active drugs was studied. In 7 of these cases the other drug present was methadone, and in the remainder dihydrocodeine, morphine, propoxyphene, amitriptyline, meprobamate, cyclizine and dipipanone, diphenhydramine and methaqualone.Amitrityline, methadone, cyclizine and dipipanone, methaqualone and diphenhydramine appeared to modify the distribution of amylobarbitone and quinalbarbitone. Likewise, the barbiturates seemed to alter the distribution of amitriptyline, propoxyphene and, in one instance, methadone.     

A survey of reported synthesis of methaqualone and some positional and structural isomers.

Methaqualone (2-methyl-3-o-tolyl-4(3H)-quinazolinone) is the illicit synthetic drug of choice amongst South African drug users. Historically police and forensic investigation has proven that all methaqualone seized by the South African Police Service originates from illicit manufacturing sites both inside, and outside South Africa's borders. From a drug enforcement, and forensic point of view it is, thus, of utmost importance that the various synthetic routes available to the illicit "chemist" are fully documented and understood. This is a prerequisite for effective illicit laboratory investigation, as well as chemical and precursor monitoring. This paper gives a brief introduction to the current status with regard to methaqualone use and production in South Africa, as well as an extensive review of the synthesis of methaqualone and selected isomers reported since 1946. A table summarizing synthetic routes reported in 32 reference sources is provided.     

Ethanol, marijuana, and other drug use in 600 drivers killed in single-vehicle crashes in North Carolina, 1978-1981

Although the use of ethanol, marijuana, and other drugs may be detrimental to driving safety, this has been established by direct epidemiological evidence only for ethanol. In this study, the incidences of detection of ethanol (and other volatile substances), delta-9-tetrahydrocannabinol (THC), barbiturates, cocaine and benzoylecgonine, opiates, and phencyclidine were determined in an inclusive population of 600 verified single-vehicle operator fatalities that occurred in North Carolina in 1978 to 1981. The incidence of detection of amphetamines and methaqualone were determined for drivers accepted for study during the first two years (n = 340) and the last year (n = 260), respectively. Blood concentrations of 11-nor-deta-9-tetrahydrocannabinol-9-carboxylic acid (9-carboxy-THC) were determined in THC positive drivers. EMIT cannabinoid assays were performed on blood specimens from all drivers accepted for study during the third year, and the feasibility of using the EMIT cannabinoid assay as a screening method for cannabinoids in forensic blood specimens was investigated. The incidence of detection of ethanol (79.3%) was far greater than the incidences determined for THC (7.8%), methaqualone (6.2%), and barbiturates (3.0%). Other drugs were detected rarely, or were not detected. Blood ethanol concentrations (BECs) were usually high; 85.5% of the drivers whose bloods contained ethanol and 67.8% of all drivers had BECs greater than or equal to 1.0 g/L. Drug concentrations were usually within or were below accepted therapeutic or active ranges. Only a small number of drivers could have been impaired by drugs, and most of them had high BECs. Multiple drug use (discounting ethanol) was comparatively rare. Ethanol was the only drug tested for that appears to have a significantly adverse effect on driving safety.     

The analysis of illicit methaqualone containing preparations by gas chromatography-mass spectrometry for forensic purposes

A validated gas chromatographic-mass spectrometric method for quantitative analysis of methaqualone (MTQ) in illicit preparations is reported. The method proved to have a coefficient of variation of below 5%. Four batches of seized tablets, two pairs with similar imprints, were analyzed. It was found that the average MTQ concentration in all four batches of tablets differed significantly (p = 0.01) rendering it impossible to conclude that, on the basis of MTQ concentration alone, the batches with a similar logo originated from the same manufacturer or manufacturing batch. Conversely, it can be said that in this case, the four batches originated from either different clandestine laboratories or manufacturing batches.     

Wide-bore capillary column gas chromatography in toxicological analysis of biological samples from multidrug overdoses fatalities

Fatalities from multidrug overdoses account for 25% of the total number of all poisoning fatalities and as such deserve greater attention from researchers than single drug overdoses. High resolution, good sensitivity, and repeatability provided by gas chromatography (GC) with wide-bore capillary silica and glass columns make GC particularly useful for identification and quantitative analysis of drugs in toxicological screening of autopsy specimens. Results of toxicological findings in three deaths from multidrug overdoses (methaqualone, doxepine, methotrimeprazine, pernazine-aspirin, paracetamol, codeine-morphine, diazepam) occurring in routine medical practice are reported.     

Metabolite sensitivity in the methaqualone radioimmunoassay.

Recent literature reflects the increased use of RIA as a qualitative and quantitative tool. This study exemplifies the problems that may arise when this technique is used for quantitation. Caution must be exercised, and a physiological and toxicological understanding of each particular drug is essential to provide credible results. It is evident that the sensitivity and ease of the RIA method for methaqualone makes it invaluable as a screening test, but confirmation and quantitation of this drug must remain with those methods that can quantitate each metabolite.     

Occurrence of barbiturate, benzodiazepine, meprobamate, methaqualone and phenothiazine in car occupants killed in traffic accidents in the south of Sweden

An investigation of the following psychoactive drugs: barbiturate, benzodiazepine, meprobamate, methaqualone and phenothiazine, was performed on all automobile occupants killed in accidents in southern Sweden during 1977 and 1978. Of 122 drivers and 55 passengers analysed, low concentrations of these drugs were found in nine drivers and in five passengers. Thus, 7.3% of the drivers were driving under the influence of drugs and, of these, two drivers (1.6% of all analysed drivers) were also inebriated. Twenty-three per cent of the drivers were inebriated only. According to the circumstances in the accidents and the number of drivers whose analyses proved positive, drug influence seldom seems to be the cause of fatal traffic accidents.     

The isolation and identification of precursors and reaction products in the clandestine manufacture of methaqualone and mecloqualone

Abuse of the hypnotic quinazolinone is well recognized and increasing. Clandestine laboratories producing methaqualone (2-methyl-3-ortho-tolyl-4(3H) quinazolinone) and mecloqualone (2-methyl-3-ortho-chlorophenyl-4(3H) quinazolinone) have been discovered throughout the United States. These laboratories utilize one of many synthesis routes to produce the illicit quinazolinone. Frequently, the clandestine chemist has little, if any, formal education in chemistry; does not keep notes; and does not label flasks and beakers containing solutions. The forensic chemist may be asked to analyze unmarked reaction mixtures that were seized in a clandestine laboratory raid. As a result, a rapid method of isolation and identification of the precursors and products of such a mixture is presented.