灌服摇头丸兔组织中甲基安非他明及其代谢物检验

苯丙胺类药品主要包括安非他明 (AM )、甲基安非他明 (MAM )、 3,4 亚甲二氧基安非他明 (MDA)、3,4 亚甲二氧基甲基安非他明 (MDMA )等 ,为人工合成的具有成瘾性的精神兴奋药 ,属违禁毒品 ,主要被制成摇头丸供吸毒者服用[1] 。在我国缴获的摇头丸中 ,多含有甲基安非他明。因此 ,在生物体内检测出甲基安非他明 (methamphetamine ,MAM )及其代谢物安非他明 (amphetamine ,AM)是服用摇头丸的重要依据。本文作者给兔灌服摇头丸 ,用液液微萃取法[2 ,3] 提取其组织检材中甲基安非他明及其代谢物安非他明[2 ,3] ,GC/NPD测定 ,研究甲基安…     

LC-MS/MS法测定血液中卡马西平及其代谢物

目的 建立LC-MS/MS法测定血液样品中卡马西平及其代谢物10,11-二氢-10,11-环氧卡马西平和10,11-二氢-10-羟基卡马西平的方法。方法 以1-丁基-3-甲基咪唑六氟磷酸盐离子液体为萃取剂处理血液样品,通过超声辅助萃取,采用ZORBAX Eclipse Plus C18,95?色谱柱分离,流动相A为含0.1%甲酸、10 mmol/L乙酸铵的水溶液,流动相B为混合有机溶剂(V_乙腈∶V_甲醇=2∶3),梯度洗脱,流速1.00 mL/min,采用电喷雾离子源、正离子模式,多反应监测模式进行检测。结果 血液样品中卡马西平及其代谢物10,11-二氢-10,11-环氧卡马西平和10,11-二氢-10-羟基卡马西平在相应范围内线性关系良好,相关系数(r)均大于0.995 6,检出限分别为3.00、0.40和1.30 ng/mL,定量限分别为8.00、1.00和5.00 ng/mL,提取回收率为76.00%～106.44%,日内和日间精密度均小于16%。采用本方法从死亡案件的血液样品中检出卡马西平和主要代谢产物10,11-二氢-10,11-环氧...     

生物样品中AM、MAM、MDA、MDMA及其代谢物的分析研究（综述）

本文介绍了常见安非他明类兴奋利AM(安非他明)、MAM(甲基安非他明)、MDA(3,4-亚甲二氧基安非他明)、MDMA(3,4-亚甲二氧基甲基安非他明)的毒性、中毒症状以及近十年生物样品中原体和代谢物分析方法的研完成果,重点介绍GC、GC/MS和HPLC的检测方法。     

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。     

尿中氯胺酮及其代谢物盘鉴和GC/MS/SIM测定

目的 研究尿中氯胺酮(KET)及其代谢物去甲基氯胺酮(NKET)的盘鉴(Disk SPE)。方法 用含有化学键合C18和强酸型强阳离子交换(SCX)基团的萃取柱SPEC.C18 AR/MP3萃取,加入萃取柱前的尿样用0.1mol/L磷酸盐缓冲溶液(pH 6)稀释,洗脱溶剂为含2％(v/v)氨水的乙酸乙酯;以2,4,6-三硝基甲苯(TNT)为色谱内标,GC/MS/SIM检测。结果 在加标量为0.5μg/mL、2μg/mL和6μg/mL的控制尿样中,KET和NKET的平均回收率分别为91.5％和79.9％,6次测定的RSD均为8.7％;线性范围0.02-8μg/mL,线性相关系数分别为0.9819和0.9964;检出限(S/N=3)分别为6ng/mL和4ng/mL;总离子色谱图背景低,杂质少。同一根萃取柱重复使用8次以上未见性能下降;嫌疑尿样中检出KET和/或NKET,和常规的液液萃取结果相符。结论 该方法适用于尿中KET和NKET的同时测定。     

溴敌隆及其代谢物-苄叉丙酮在犬体内的死后分布

目的研究溴敌隆及其代谢物-苄叉丙酮在中毒致死犬体内死后分布规律,为溴敌隆中毒检材的采取提供实验依据。方法分别经口给予犬2倍和4倍LD_(50)溴敌隆,待其死亡后迅速解剖取材,气相色谱-质谱联用法测定心血、外周血、尿、胆汁、心、肝、脾、肺、肾、脑、左下肢肌、膀胱、胃、胃内容、胰等脏器和体液中溴敌隆和代谢物-苄叉丙酮的含量。结果犬经2倍和4倍LD_(50)溴敌隆灌胃染毒后3d开始出现出血症状,(178.40±20.94)h后死亡。溴敌隆和代谢物-苄叉丙酮在各组织脏器及体液中的死后分布为:溴敌隆2LD_(50)组溴敌隆:胆汁尿、肝、心、肾心血、外周血、脾、肺等;苄叉丙酮:胆汁、尿、心血、外周血、肺、胃内容中含量高于其他脏器。溴敌隆4LD_(50)组溴敌隆:胆汁、尿肝、外周血心血、胃内容物等脏器。苄叉丙酮:胆汁、尿、肺浓度高于其他脏器。结论溴敌隆及其代谢物-苄叉丙酮在中毒致死犬体内死后分布不均匀,溴敌隆在胆汁、尿、肝脏、心血和外周血含量较高,代谢物-苄叉丙酮在胆汁、尿、肺较高。胆汁、尿、肝脏、心血、外周血可作为疑似溴敌隆中毒毒物分析的检材。     

家兔死后体内2-氨基噻唑啉-4-羧酸分布研究

目的建立家兔氰化钾灌胃给药致死动物模型,研究氰化物代谢物2-氨基噻唑啉-4-羧酸(ATCA)在家兔体内的死后分布规律。方法雄性家兔7只(体重约2.0kg~2.5kg)经口灌胃2LD50(10mg/kg)氰化钾水溶液,观察家兔反应,待家兔呼吸、心跳和反射全部消失后立即对家兔进行解剖取心、肝、脾、肺、肾、脑、睾丸、胃壁、肌肉等组织检材以及心血、玻璃体液、尿液等体液检材置于-80℃冷冻保存待检。液相色谱-串联质谱联用法测定生物检材中氰化物代谢物ATCA的含量,对其在各个组织的分布进行比较并寻找规律。结果氰化钾灌胃后家兔出现呼吸频率加快,走路乏力,癫痫大发作样抽搐,后瞳孔散大,肌肉松弛,各种反射消失,似"电击样"死亡。死亡后测得心血中氰基(CN-)平均浓度为11.81μg/ml。死后0h氰化物代谢物ATCA在家兔体内的分布如下:脾>肺>肾>肝、脑>睾丸>心血>心、胃壁>玻璃体液>右下肢肌肉>尿。结论大剂量氰化物中毒致死后其代谢物ATCA在家兔体内分布不均匀,在脾中最高,尿中最低。在疑似氰化物中毒致死案件的法医学鉴定中,除采取心血外,还应全面正确采集分布量较高的脾、肺、肾和肝组织进行氰化物代谢物ATCA的定性定量分析。     

血液1-(3-三氟甲基苯基)哌嗪和1-(3-氯苯基)哌嗪检验

目的建立血液中1-(3-三氟甲基苯基)哌嗪(TFMPP)、1-(3-氯苯基)哌嗪(m CPP)的检测方法,并用于实际案件检验。方法 Zn SO4沉淀蛋白后,在p H11条件下,用氯仿/异丙醇(4/1,v/v)提取,采用GC/MS与GC/NPD分析。结果 TFMPP、m CPP回收率均在90%以上,在0.25~20μg/m L浓度范围内线性关系良好,r2为0.999 9,最低检测限为0.135μg/m L。结论本方法回收率高,操作简便,可用于血液中TFMPP、m CPP的提取检测。     

2′-氯地西泮在大鼠体内分布及代谢降解规律研究

目的研究2′-氯地西泮及其代谢物(地洛西泮、氯甲西泮、劳拉西泮)在大鼠体内分布及代谢规律,为2′-氯地西泮相关案件的检验提供实验数据。方法40只SD大鼠随机分为4组,禁食12h,按2.625mg/kg 2′-氯地西泮灌胃给药,第一组给药后不同时间点经大鼠尾静脉采血,第二组为采血空白对照组,第三组给药30min后处死,取心、肝、肺、肾、脑、睾丸,经乙酸乙酯液液萃取后用高效液相色谱-三重四极杆质谱检测2′-氯地西泮及代谢物含量,第四组为分布空白对照组。结果2′-氯地西泮进入体内后,迅速代谢分布,在20min内达到血液最高浓度。2′-氯地西泮及代谢物在各器官中的分布特点为:肝>脑>心脏>肾>睾丸>肺。结论经灌胃2′-氯地西泮进入大鼠体内后,监测2′-氯地西泮及其代谢物在大鼠体内的分布及降解规律可以为2′-氯地西泮相关案件的检验鉴定提供参考依据。     

超声辅助离子液体萃取-高效液相色谱串联质谱法测定全血中卡马西平

目的建立超声辅助离子液体-分散液液微萃取-高效液相色谱串联质谱法(high performance liquid chromatography-tandem spectrometry,HPLC-MS/MS)测定全血中卡马西平(carbamazepine,CBZ)的方法。方法经筛选后以1-丁基-3-甲基咪唑六氟磷酸盐(1-butyl-3-methymidazolium hexafluoro-phosphate,[Bmim][PF6])为萃取剂,在空白血液中添加卡马西平和内标物双氢卡马西平(10,11-dihydrocarbamazepine,CBZ-DiH),通过超声辅助离子液体对其萃取后,采用ZORBAX Eclipse Plus C18色谱柱分离,流动相A为含0.1%甲酸、10mmol/L乙酸铵的水,流动相B为混合有机溶剂(乙腈‥甲醇=2‥3,体积比),流速1mL/min,采用电喷雾离子源正离子模式(ESI+),多反应监测模式(MRM)进行检测。结果血液中卡马西平的线性范围为8.00~300.00ng/mL,R2大于0.995,最低检出限为3.00ng/mL,最低定量限为8.00ng/mL,提取回收率大于80%,日内和日间精密度均小于20%。采用本方法从实际案件的血液样品中检出卡马西平,浓度为2.71μg/mL。结论本研究建立的全血中卡马西平的检测方法,具有环境友好、快速、富集效果好、灵敏度高、有机溶剂消耗小的优点,可应用于卡马西平相关案件的法医学鉴定。     

N-cyanomethyl-N-methyl-1-(3',4'-methylenedioxyphenyl)-2-propylamine: an MDMA manufacturing by-product

This paper describes the structural elucidation of a compound produced during the synthesis of 3,4-methylenedioxymethylamphetamine (MDMA) via the reductive amination of 3,4-methylenedioxyphenyl-2-propanone (3,4-MDP-2-P) with methylamine and sodium cyanoborohydride. The compound was isolated from MDMA by column chromatography, proton and carbon nuclear magnetic resonance spectroscopy, LC/mass spectrometry, and total synthesis were used to identify the compound as N-cyanomethyl-N-methyl-1-(3',4'-methylenedioxyphenyl)-2-propylamine. This compound has been identified as a potential synthetic route marker for the reductive amination of 3,4-MDP-2-P with methylamine and sodium cyanoborohydride and as such it should prove valuable to forensic scientists engaged in profiling illicit drugs. Profiling MDMA can provide useful information to law enforcement agencies relating to synthetic route, precursor chemicals and reagents employed and may be used for comparative analyses of different drug seizures. This paper also describes the structural elucidation of the analogous methylamphetamine synthetic route marker compound, N-cyanomethyl-N-methyl-1-phenyl-2-propylamine, produced during the reductive amination of phenyl-2-propanone using methylamine and sodium cyanoborohydride.     

杀虫双的检验和质谱解析

本文用气相色谱/质谱联用方法检验杀虫双,并解析杀虫双的质谱图.     

Methyl 3-[3',4'-(methylenedioxy)phenyl]-2-methyl glycidate: an ecstasy precursor seized in Sydney, Australia

Five 44 gallon drums labeled as glycidyl methacrylate were seized by the Australian Customs Service and the Australian Federal Police at Port Botany, Sydney, Australia, in December 2004. Each drum contained a white, semisolid substance that was initially suspected to be 3,4-methylenedioxymethylamphetamine (MDMA). Gas chromatography-mass spectroscopy (GC/MS) analysis demonstrated that the material was neither glycidyl methacrylate nor MDMA. Because intelligence sources employed by federal agents indicated that this material was in some way connected to MDMA production, suspicion fell on the various MDMA precursor chemicals. Using a number of techniques including proton nuclear magnetic resonance spectroscopy ((1)H NMR), carbon nuclear magnetic resonance spectroscopy ((13)C NMR), GC/MS, infrared spectroscopy, and total synthesis, the unknown substance was eventually identified as methyl 3-[3',4'(methylenedioxy)phenyl]-2-methyl glycidate. The substance was also subjected to a published hydrolysis and decarboxylation procedure and gave a high yield of the MDMA precursor chemical, 3,4-methylenedioxyphenyl-2-propanone, thereby establishing this material as a "precursor to a precursor."     

过敏性休克死亡体内血栓素B_2含量变化的研究

本研究采用非平衡法,对青霉素和血清过敏性休克致死机体的血浆、肺、脾和肾中血栓素B_2(Thromboxane,TXB_2)进行放射免疫分析(RIST)。正常对照组血浆中TXB_2含量是9.63±1.77(ng/ml),实验组休克前是9.264±3.01(mg/ml),两者P>0.05。青霉素休克组30.36±10.72(ng/ml);血清休克组40.10±6.51(ng/ml),与对照及休克前相比均P<0.01。对照、青霉素和血清过敏性休克肺中TXB_2依次为:89.90±6.57、171.96±18.07和187.70±18.89(ng/g)(P<0.01)。脾中依次为:68.334±10.09、137.68±15.97和173.72±18.75(ng/g)(P<0.01)。肾中依次为:73.89±5.05、128.30±19.99和152.15±17.77(ng/g)(P<0.01)。过敏性休克致死的机体置室温6或12h,或冰箱48h后,不明显影响TXB_2的检测。研究者认为:发生过敏性休克时,血栓素系统发生剧烈变化,表现为血和脏器中TXB_2的增加,可为确定过敏性休克死亡提供一个重要的生化指标。     

短串联重复位点ACTBP2(SE33)的扩增片段长度多态性研究

应用变性聚丙烯酸胺凝胶电泳（dn－PAGE）结合银染色技术对短串联重复（STR）位点ACTBP2（SE33）的扩增片段长度多态性（Amp－FLPs）进行了研究。在210名无关中国个体中观察到了25个等位基因，等位基因频率分布在0．007～0．093之间。基因型的分布符合Hardy－Weinberg定律，个体识别能力（DP）值为0．99，杂合度（H）为98．7％。七个家系分析的结果表明，该位点的遗传符合孟德尔遗传法则，未观察到变异。对几种常见的法医物证检材的分析表明，该分型系统对DNA降解放为严重的检村适用性强，而且灵敏度高（0．5ng），适合于法医学实际应用。     

A micromethod for the isolation of drugs from blood using amberlite XAD-2

The extraction of drugs from small blood samples (1 ml or less) for subsequent quantitative determination is described. Isolation was carried out by adsorption of the drugs to Amberlite XAD-2 resin utilizing a batch procedure that enabled the simultaneous extraction of up to 200 samples in approx. 5 hours. A new desorption technique yielded extracts of high purity that could be used directly for gas chromatographic or radioimmunological determinations, even if hemolyzed or putrid blood was to be examined. The following 26 substances were quantitated after addition to postmortem blood speciments at concentrations of 1-10 microgram/ml: tilidine, diphenhydramine, dibenzepine, imipramine, chlorpromazine, amphetamine, pentazocine, phenacetin, methaqualone, meprobamate, parathion, diazepam, digoxin, beta-methyldigoxin, carbromal, glutethimide, amobarbital, pentobarbital, cyclobarbital, phenobarbital, diphenylhydantoin, carbutamide, tolbutamide, glycodiazin, tolazamide and chlorpropamide. Thereby recoveries of 60-100% could be achieved. The reproducibility of the procedure was satisfactory as demonstrated by coefficients of variation of 3.7-8%.     

胶体金免疫层析一步法快速检测G1m(3)因子

建立一种简便快速的胶体金免疫层析一步法 ,用于检测 G1m(3)因子。采用柠檬酸三钠还原法制备胶体金颗粒 ,标记抗人 G1m(3)单克隆抗体 ,研制出抗人 G1m(3)因子免疫层析检测试剂盒。样品的 G1m(3)因子 ,与测试条上的金标记抗体结合后沿着反应膜移动 ,再与膜上固相抗体结合形成肉眼可见的红色反应带。使用该方法可检出 10万倍稀释的血清样品 ,整个试验只需 5 min完成。对常见的 2 3种动物血 (痕 )检验 ,未出现交叉反应。在 10 0例样品的检测中 ,本方法的检测结果 ,与 Dot- EL ISA的检测结果的符合率为 10 0 %。该方法适用于法医物证快速检验。     

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.     

Cleavage of 2-phenylpropan-1-ol and 2-phenylpropan-2-ol-glucuronide, 2 metabolites of isopropylbenzol (Cumol)

The behaviour of 2-phenyl-1-propanol (I) and 2-phenyl-2-propanol (II) and their glucuronides with HCl has been investigated. While I shows a high acidic constancy, II undergoes a partial conversion into 2-phenylpropane (III) which itself yields numerous products. The glucosidic bond of glucuronide I is quantitatively split by 10.0% HCl, whereby an aglucone yield of nearly 100% is obtained. The second glucuronide behaves otherwise: the recovery of II is very low (only 40% to 45%) with HCl concentrations of 1.0%-20.0%, although with 1.0% HCl 100% of the glucuronide is hydrolysed.     

反相高效液相色谱法测定人血浆中的吲哚美辛

建立血浆中吲哚美辛的高效液相色谱分析方法 ,扩大药 (毒 )物检测范围及手段 ,以适应法医学鉴定的特殊需要。以空白血浆标准添加吲哚美辛对样品处理方法、线性关系、回收率及精度进行考察 ,并以所建方法对健康受试者的血液浓度进行监测。方法的线性范围是 0 1～ 5 0 μg·ml-1,γ =0 9995 ,最小检出浓度为 0 0 2 μg·ml-1(S/N≥ 3)。日内、日间的方法精密度为 ( 1 1± 0 2 ) % (n =4)和 ( 2 7± 0 6 ) % (n =4) ,加样回收率为 97 5 %～10 4 2 %。所建方法准确、便捷、选择性好 ,可用于法医学鉴定及血液浓度监测