尿中MDMA及其代谢物的GC和GC／MS分析

考察MDMA在人体内的代谢以及建立尿中MDMA和体内主要代谢物MDA的分析方法。尿样水解后经液-液提取处理,用GC／MS（EI、PCI）和GC／FID法分析。人摄入MDMA后尿中MDA和原体MDMA比约为0．10～0．14。GC／MS／SIM和GC／FID法的最低检出限为2ng／ml和50ng／ml,回收率大于85％,变异系数小于10％。该法简便快速、灵敏度高、结果可靠,可用于MDMA滥用者的尿样鉴定。MDA／MDMA浓度比可作为评判毒分结果的参考指标。     

气相色谱质谱联用法检测大鼠尿液中2C-B及其代谢物

目的研究4-溴-2,5-二甲氧基苯乙胺（2C—B）在大鼠体内的代谢物以及代谢途径。方法取Wistar大鼠3只,以2C-B灌胃,收集24h内尿液,用B葡萄糖醛酸酶水解,Oasis HLB柱固相提取,DB-35MS柱分析,气相色谱质谱联用检测。结果从大鼠尿液中检出6种2C-B的代谢产物,分别为：4-溴-2-羟基-5-甲氧基苯乙醇、4-溴-2,5-二甲氧基苯乙醇、4-溴-2-羟基-5-甲氧基苯乙酸、4-溴-2,5-二甲氧基苯乙酸、1-乙酰氨基-2-（4-溴-5-羟基-2-甲氧基苯）乙烷和1-乙酰氨基-2-（4-溴-2-羟基-5-甲氧基苯）乙烷。未检出2C—B原药。结论2C-B在大鼠尿液中主要以代谢物形式存在,其在大鼠体内至少仔在两种代谢途径：第一种是2C—B的2位和5位氧上去甲基后氨基被乙酰化;第二种是2C—B去氨基生成醛,接着被还原或氧化生成醇和羧酸。     

用GC／ECD方法分析海洛因中毒尿液吗啡代谢物

目的　考查尿检材中海洛因的代谢物吗啡和单乙酰吗啡的液液萃取条件、三氟乙酰化和气相色谱电子捕获检测 (GC/ECD)条件。方法　以烯丙吗啡为内标 ,氯仿∶异丙醇 (9∶1)为液相萃取剂萃取尿中的吗啡和单乙酰吗啡 ,采用MBTFA衍生化 (三氟乙酰化 ) ,GC/ECD检测。结果　尿中加样相对回收率吗啡 89% ,单乙酰吗啡 75 % ,最小检测量吗啡 5 0ng ,单乙酰吗啡 10 0ng。通过实验兔的中毒实验 ,对尿检材进行了分析。 结论　所建立的萃取与检测方法分析海洛因中毒尿检材中的吗啡准确、灵敏 ,可用于海洛因的吸毒检验     

GC/MS determination of zolpidem in postmortem specimens in a voluntary intoxication

An ingestion of an unknown quantity of Ivadal (zolpidem) tablets in a case of drug abuse is described. The authors report a new and fast method of analysing and determining the zolpidem concentration in postmortem specimens. Quantitation of zolpidem was performed by ethyl acetate extraction from alkalinized body fluids before GC/MS analysis. The analyses were performed without any complex sample clean-up steps and with little sample material. Postmortem concentrations of zolpidem in body fluids are given. The proposed method is a rapid procedure of analysis in cases of deliberate poisoning with the sedative-hypnotic drug, zolpidem.     

中毒致死者体内芬氟拉明的GC/NPD,GC/MS法测定

建立了生物检材中芬氟拉明的定性定量分析方法。体液及脏器组织经有机溶剂提取后 ,用GC/MS法进行药物筛选、定性 ,生物检材中的芬氟拉明浓度用4 -苯丁胺作内标、GC/NPD法测定。测得芬氟拉明中毒致死者的血液、尿液、肝等组织中浓度分别为7.8μg/ml、64.2μg/ml、31.3μg/g。并对尸体解剖所见及方法可行性进行讨论     

Determination of methadone in urine using ion trap GC/MS in positive ion chemical ionization mode

Methadone is a potent analgesic and sedative. It is widely used in the treatment of heroin addiction and is often encountered in forensic specimens. In electron impact (EI) gas chromatography/mass spectrometry (GC/MS) mode, methadone produces predominantly a m/z 72 ion, which is not sufficiently characteristic for identification. Determination of the molecular ion, which can be achieved using chemical ionization (CI) provides diagnostic information and better identification of the drug. This paper describes the development of a positive ion CI GC/MS procedure, using a liquid reagent gas and ion trap instrumentation, for the determination of methadone and its metabolites in urine. CI generally produces a single molecular ion spectrum, but optimization of the reagent gas parameters increases the fragmentation of the molecule, allowing determination of ion ratios if required. The procedure is sensitive, diagnostic and is currently in routine use in our laboratory.     

微波衍生化和GC/MS/MS技术分析血、尿中的吗啡

目的建立了血、尿等生物检材中海洛因代谢产物吗啡的定性分析方法。方法以丙酸酐为衍生化剂,采用微波衍生化技术结合GC/MS/MS进行分析。结果当CID电压为0.9V时,衍生化物的母离子与子离子碎片信息丰富,碎片为m/e268、324、342。结论此方法科学、准确,灵敏度高,能满足吸食海洛因类、吗啡类毒品人员的生物检材的检验要求。     

顶空固相微萃取与气质联用快速检测尿液中氯胺酮及去甲基氯胺酮

目的建立利用顶空固相微萃取（HS／SPME）结合气相色谱／质谱联用技术（GC／MS）快速检测吸毒人员尿液中氯胺酮（KT）及其主要代谢物去甲基氯胺酮（NK）的方法。方法样品瓶中加入尿样、6mol／L氢氧化钠溶液、固体氯化钠、SKF525A（内标），85℃下加热搅拌，用100μm聚二甲基硅氧烷（PDMS）萃取头顶空萃取10min，GC／MS（EI-SIM）检测。结果尿液中NK和KT浓度在0．1～2．0μg／ml范围内呈现线性关系，相关系数分别为（r^2）0．9991和0．9945，检测限（D／N=3）分别为0．87ng／ml和2．76ng／ml，定量限（S／N=10）分别为2．90ng／ml和18．52ng／ml。1ml尿液加标600ng，NK回收率在85．5％～110．1％，RSD〈13．2％（n=6）；KT回收率在77．5％～109．6％，RSD〈511．99％（n=6）。结论建立的方法简单、快速、灵敏、准确，适合尿液等生物检材中NK及KT的快速定性定量分析。     

内标法固相提取-GC/MS检测海洛因吸食者尿液中代谢物

本文建立了以SKF-525A作内标、GDX－301作固相提取剂、用GC／MS方法测定海洛因吸食者尿液中代谢物浓度的方法。系统考查了吗啡、单乙酰吗啡的提取回收率、线性关系等指标。所建立的方法对吗啡和单乙酰吗啡的回收率均大于80％;最小检测浓度小于0.1μg／ml;用代谢物特征离子与内标物特征离子峰高比法测定吗啡与单乙酰吗啡的浓度,在每ml尿添加0．25μg～250μg范围内,二者均有良好的提取线性关系。并对几例海洛因滥用者的尿液进行了检测。     

SPE-GC／MS法检测大鼠尿中尼美西泮及其代谢物

目的检测尼美西痒阳性大鼠尿液中的代谢物。方法2只Wistar大鼠分别喂食半粒尼美西泮药丸，收集24h内尿液，用B葡萄糖醛酸酶水解，Oasis@HLB柱固相提取，以DB．35Ms柱为分离柱，气相色谱质谱联用法检测。结果从大鼠尿液中检出尼美西泮的4种代谢物：7-乙酰氨基尼美西泮、7-乙酰氨基硝基安定、7-氨基尼美西泮和2-氨基-5-硝基苯基苯甲酮及少量尼美西泮原体。结论尼美西泮在大鼠体内易代谢，在尿液中的主要代谢物为7-乙酰氨基尼美西泮和7-乙酰氨基硝基安定。     

固相微萃取（SPME）GC／MS、GC／MS／MS法检测环境水中的有机磷杀虫剂

目的　通过对固相微萃取 (SPME)条件的优化、筛选实验 ,建立环境水中有机磷杀虫剂的快速检验方法。方法　收集 17种有机磷杀虫剂 ,使用SPME并结合GC/MS、GC/MS/MS检验方法。结果　该方法简便、灵敏、迅速、可靠 ,样品利用率高 ,最低检测浓度为 0 .0 1～ 10 0 pg/ml,在痕量范围 0 .1～ 10ng/ml内线性回归好(相关系数r达 0 .99以上 )。结论　实际应用效果理想 ,有望成为公安、环保、检验检疫的农残及毒物分析中的一种快速有效的分析方法。     

丁丙诺啡的检验

目的建立检验丁丙诺啡的方法。方法用气质联用仪与高效TLC法进行定性分析。结果丁丙诺啡在展开剂苯∶正己烷∶二乙胺=40∶10∶10时,Rf值为0.55;环己烷∶丙酮=1∶1时,Rf值为0.35;质谱图保留时间为19.617min。结论本方法操作简便、准确,适合办案。     

液相色谱质谱联用测定乌头碱在大鼠体内代谢产物

目的鉴定乌头碱在大鼠体内的主要代谢产物。方法灌胃给予雄性大鼠1.0mg/kg乌头碱后,收集24h尿液,固相萃取法提取,液相色谱-质谱法测定乌头碱及其代谢物。结果经与空白组对照发现给药后大鼠尿样中除乌头碱原体外还有4种代谢产物,并分别测得其准分子离子峰及其各级碎片离子。结论经与对照品比较及质谱断裂规律推断4个代谢产物分别为中乌头碱、16-O-去甲基乌头碱、16-O-去甲基中乌头碱、苯甲酰乌头碱。     

GC/MS测定尿液中氯胺酮含量不确定度评定

目的评定气相色谱—质谱法（GC/MS）测定尿液中氯胺酮含量的不确定度。方法依据不确定度评定的指导性文件,从测定程序分析了不确定度的来源,量化不确定度分量,计算检测结果的合成标准不确定度和扩展不确定度。结果尿液检材中测定结果平均值为0.257μg/mL的扩展不确定度为0.016μg/mL。结论尿液中氯胺酮含量的不确定度主要来源于标准品纯度和标准曲线。     

Chronological study of diazinon in putrefied viscera of rats using GC/MS, GC/EC and TLC

A qualitative and qualitative weekly study of diazinon in experimental rats after a lethal dose is described. GC/MS and TLC were used for qualitative, and GC/EC for quantitative analysis. The replicate content of diazinon in stomach and intestine (S/I) revealed a high rate of decrease during the first month. The liver (L) content fluctuates through a general trend of decrease. Immediate post-mortem content of 34.5 mg in summer and 94 in winter was found in S/L samples, while it was 0.79 and 0.63 respectively for L-samples. The respective remaining amount after 2 months was 1. 16, 4.40 (S/I), 0.61 and 0.66 mg (L). A round figure of 4% remains in S/L samples. The chronological plots indicate the possibility of detection at longer periods. Interpretation of data is outlined regarding relative contents of organs and the factors affecting persistence of diazinon in putrefied viscera.     

电场促进下的固相微萃取-GC/MS法测定尿中的苯丙胺类兴奋剂

目的采用电场促进下的固相微萃取(EE-SPME)-GC/MS分析方法,对尿中苯丙胺(AM)、甲基苯丙胺(MA)、3,4-(亚甲二氧基)苯丙胺(MDA)、3,4-(亚甲二氧基)甲基苯丙胺(MDMA)和3,4-(亚甲二氧基)乙基苯丙胺(MDEA)5种苯丙胺类兴奋剂进行定性定量分析。方法通过向萃取纤维附近引入阴极,促使样品溶液中的目标物阳离子向萃取纤维附近迁移,从而提高了PDMS涂层在温和条件下对苯丙胺类兴奋剂的萃取效率。对EE-SPME条件进行优化,以4-苯基丁胺(4-PBA)为内标,在气-质仪联用选择离子检测(GC/MS/SIM)模式下进行定性定量分析。结果本方法的检出限为0.1～1.2ng/mL,线性范围为1～200ng/mL,相关系数为0.990～0.997,三个加标水平(5、50、100ng/mL)下的回收率为86%～110%,精密度可达3.6%～8.7%。结论该方法灵敏、准确、对环境绿色友好,并且操作简便。     

The detection of 6-monoacetylmorphine in urine, serum and hair by GC/MS and RIA

6-Monoacetylmorphine (6-MAM) is a good indicator for the intake of heroin and can be detected in blood, urine and hair of heroin users. A new radioimmunoassay (RIA) designed specifically for 6-monoacetylmorphine (6-MAM) was tested for its usefulness for the quantitation of the drug in urine, serum and hair. Its cross-reactivity with heroin and its metabolites, and related compounds was also determined. Eighty-nine hair, six serum and 25 urine samples where 6-MAM had been previously identified by GC/MS were analysed for 6-MAM with the new RIA kit. A good correlation existed between the GC/MS and RIA results for the hair samples. However, the amount of 6-MAM found in serum and urine differed considerably between the two methods. This difference could be explained by the cross-reactivity of the antibody with morphine and morphine-6-glucuronide, which are present in much larger amounts in serum and urine, than in hair. To evaluate a new rationalisation procedure, some hair samples were split into two portions after incubation. One part was analyzed for 6-MAM by RIA, and the other portion by GC/MS.     

利用GC／MS检验致幻剂麦角酰二乙胺

目的建立检验致幻剂麦角酰二乙胺的方法。方法用气相色谱与质谱联用仪(GC/MS)进行定性分析。结果麦角酰二乙胺质谱图保留时间为19.683min。结论该方法用于检案简单、可靠。     

Comparative analysis of gamma-hydroxybutyrate and gamma-hydroxyvalerate using GC/MS and HPLC

This paper describes two analytical techniques used to separate and quantify gamma-hydroxybutyrate (GHB) and gamma-hydroxyvalerate (GHV). The first technique was a N,O-bis(trimethylsilyl)triflouro-acetimide-trimethylchlorosilane derivatization, followed by gas chromatography/mass spectrometry analysis using an HP-5 capillary column at a rate of 1.0 mL/min with a run time of 9.25 min. This technique was found to be sensitive (LOD 1 pg on column) and gave a low average error (5%) in a beverage study. When supplemented by a surrogate spike, the method yielded 97% analyte recovery from beverages. The second technique was high-performance liquid chromatography/UV (HPLC/UV) using a C-18 column with a (20:80% v/v) methanol:dibasic phosphoric buffer (10 mM, pH 3) at a rate of 1.00 mL/min with a run time of 7.5 min. UV detection occurred at 254 nm. This method was found to be less sensitive (LOD 0.05 microg on column) for direct analysis of aqueous samples. To remove interferences seen in the beverage study, a liquid-liquid extraction before HPLC analysis was tested. However, a decreased sensitivity (LOD 100 microg on column) and irreproducible peak profiles resulted.