苯丙胺类药物的气相色谱及气质联用检测

本文报道苯丙胺等１１种类似药物，用气相色谱及气质联用方法进行同时分离、检测和鉴定。志愿者尿样中母体药物及其代谢物的研究，可准确判断未知尿样中此类药物的存在。     

人尿中脱氢睾酮代谢物的GC/MS分析

本文用GC/MS方法,对人尿中脱氢睾酮(boldenone)代谢物进行了研究。志愿者口服20 mg脱氢睾酮后,收集阳性尿。尿样经过包括XAD-2树脂柱吸附、酶水解、有机相萃取及三甲基硅烷衍生化反应的预处理后,用毛细管气相色谱与质谱检测器联用进行分析,鉴定了脱氢睾酮的几个主要代谢物和它们的代谢模式;总结了兴奋剂检测中具有意义的代谢物及其碎片离子;对收集的阳性尿中脱氢睾酮浓度进行测定;对预处理方法的回收率进行了研究。     

液相色谱-串联电喷雾离子阱质谱法鉴定大鼠尿液中药根碱代谢物

目的研究药根碱在大鼠体内的主要代谢产物。方法健康大鼠尾静脉注射12 mg·kg^-1药根碱，收集0～72 h的尿样，尿样经C₁₈小柱固相萃取分离纯化后，经液相色谱-串联电喷雾离子阱质谱(LC-ESI/ITMSⁿ)分析鉴定其中的代谢物。代谢物的结构鉴定主要依据各代谢物与原药的一级质谱电离规律和二级或三级质谱裂解规律间的关联性。结果在大鼠尿样中检测到7种I相代谢产物(如原药的脱氢、脱甲基、羟基化代谢物)及11种II相代谢产物(如甲基化轭合物和葡糖醛酸轭合物)。结论本方法用于大鼠尿样中药根碱的代谢物研究不仅操作简单、快速，而且灵敏度高、专属性强。     

用液相色谱-离子阱质谱联用法检测兔体液中阿普唑仑及其主要代谢产物

建立鉴别体液中阿普唑仑及其主要代谢物的高效液相色谱 电喷雾离子阱质谱联用(LC/MSn)法 .采用LC/MSn联用技术 ,检测家兔灌胃给药后血样和尿样中阿普唑仑原形药及其羟基化代谢物、葡萄糖苷酸型结合物 ,得到了它们的色谱、质谱以及特征碎片离子信息 .阿普唑仑的最低检测限小于 1ng .本法专属性强 ,可推广至其他生物检材的测定 ,尤其适用于需快速响应的临床和法医毒物分析     

气相色谱/燃烧炉/同位素比值质谱方法对尿中去氢表雄酮及其代谢物的检测

目的测定服用去氢表雄酮制剂后人尿中去氢表雄酮及其代谢物的同位素比值(¹³C与¹²C含量比值的相对值，以δ表示)进行测定，以检测尿中类固醇的来源。方法采用固相萃取、酶解、薄层色谱等方法对尿样中内源性类固醇激素进行提取、酶解游离型、分离，再经气相色谱/燃烧炉/同位素比值质谱方法测定去氢表雄酮、其代谢物内源性类固醇激素、内源性类固醇参照物的同位素比值的相对值(δ值)。将被检测物与参照物δ值之比，与判别标准比较进行来源判定。结果服用去氢表雄酮制剂后人尿中内源性类固醇激素代谢物δ值比未使用去氢表雄酮制剂正常值降低，并提示有外源性类固醇摄入。结论本法可以检测尿中去氢表雄酮或其代谢物的来源。     

HPLC-ESI-ITMSn法鉴定麻黄碱及其大鼠体内主要代谢产物

目的建立快速灵敏的LC-ESI-ITMSⁿ分析检测麻黄碱及其大鼠体内代谢物的方法。方法以麻黄碱对照品对LC-ESI-ITMS²色谱及质谱条件进行了优化，分析总结其电喷雾质谱的一级电离规律和多级质谱裂解规律，以此作为麻黄碱大鼠体内代谢物分析鉴定的依据。健康大鼠空腹灌胃麻黄碱10 mg·kg^-1，收集0~48 h的尿样，经C₁₈小柱固相萃取分离纯化后，直接采用LC-ESI-ITMSⁿ方法对尿样进行测定。结果根据生物体内药物代谢转化规律及母体药物的色谱-质谱行为规律，在尿样中鉴定出3个第I相代谢产物，未发现第II相代谢产物。结论本方法灵敏、快速、选择性高、专属性好，可用于麻黄碱的代谢产物研究。     

血、尿中安眠酮及其代谢物的测定

通过一例安眠酮中毒病人血、尿中安眠酮及其代谢物的测定,描述了用紫外光谱(uv)、气相色谱(GC)和气相色谱质谱(GC/MS)法测定安眠酮及其代谢物的系统分析方法。样品的提取净化采用液一液萃取和固相萃取两种方法,都得到了很好的结果。紫外光谱用于测定血、尿中安眠酮和其代谢物的总量;气相色谱用于测定血、尿中安眠酮原药的含量;气相色谱质谱则用于鉴定血、尿中的安眠酮及其代谢物。除安眠酮外,血、尿中共检出10种安眠酮代谢物,其中包括两种乙酰化代谢物。此法还为临床救治提供指导。     

GC-MS检测甾体同化激素类药物

本文综述了国际奥委会禁止运动员服用的甾体同化激素药物的检测方法,包括尿样净化、酶解、衍生化、气相色谱分离和选择性离子检测等主要步骤,对每一步骤所用的方法进行比较.也论讨了原料甾体药物在体内的几种代谢途径和这些药物及其代谢物的质谱裂解方式.最后给出常用的气相色谱分离条件,检测各种甾体药物的离子质荷比以及有关尿样中睾酮-表睾酮比值的规定.     

用裂解气相色谱-质谱法分析丁香油中的成分

目的研究对丁香油成分进行分离、鉴定的方法。方法采用裂解 毛细管气相色谱 质谱联用技术对丁香油成分进行分离并定性、定量。结果丁香挥发油中主要成分是丁香油酚和 β 石竹烯 ,相对含量约为 89%。 结论确定了用裂解 毛细管气相色谱 质谱联用技术进行天然植物鉴定及评价的方法。     

HPLC-MSn法鉴定葫芦巴碱及其在大鼠体内的主要代谢产物

目的建立快速灵敏的LC-MSⁿ检测葫芦巴碱及其在大鼠体内代谢物的分析方法。方法以葫芦巴碱对LC-MS²色谱及质谱条件进行优化，分析其电喷雾质谱的一级电离规律和多级质谱裂解规律，以此作为葫芦巴碱大鼠体内代谢物分析鉴定的依据。健康大鼠尾静脉注射8 mg·kg^-1葫芦巴碱，收集0～48 h的尿样，经C₁₈小柱固相萃取分离纯化后，直接采用LC-MSⁿ方法对尿样进行测定。结果根据生物体内药物代谢转化规律及母体药物的色谱-质谱行为规律，在尿样中鉴定出母药及其N-去甲基、N-去甲基环氧化产物，以及母药及其N-去甲基环氧化物的甘氨酸轭合物。结论本方法灵敏、快速、选择性高、专属性好，可用于葫芦巴碱的代谢产物研究。     

麻醉性镇痛剂及中枢神经刺激剂的分析研究

本文叙述了用高分辨气相色谱法/火焰离子化检测器,气相色谱/氮磷检测器以及气相色谱/质量选择检测器对12种麻醉性镇痛剂和2种中枢神经刺激剂的分析研究。样品用不同衍生化方法作了比较。初步结果表明:衍生化效果TFAA比MBTFA好,但与MSTFA无明显区别。本法对所有14种药物均能获得满意的分离,为筛选这些药物提供了可靠、快速而简易的方法。     

β-受体阻滞剂的分析研究

本文叙述了用高效毛细管气相色谱/氮磷检测器及气相色谱/质量选择检测器对13种β-受体阻滞剂的分析研究。样品用不同衍生化方法作了比较,初步结果表明:衍生化效果TFAA与MBTEA无很大差异;而MSTFA比上述两者效果均佳。本文的研究为β-受体阻滞剂的体液气相色谱研究提供了可行的方法。     

苯甲吗啉类药物的代谢及代谢产物的研究

本文报道苯甲吗啉类药物的气相色谱与气质联用检测方法。用HP-5890A气相色谱仪、氮专属性检测器,对服药后不同时间排尿中原型药及主要代谢产物,以内标法定量测定,绘制尿累积排泄曲线.醚提取物用三氟醋酐衍生化、气相色谱、气质联用分析比较衍生化前后保留时间及质谱数据,鉴定主要代谢产物苯甲吗啉,微量代谢产物去甲麻黄素、去甲伪麻黄素、麻黄素和伪麻黄素,方法灵敏、结果可靠,适用于此类药物的临床监测与运动员尿样检测。     

A new method for simultaneous determination of cyclic antidepressants and their metabolites in urine using enzymatic hydrolysis and fast GC-MS

A method for the simultaneous determination of six commonly prescribed cyclic antidepressants and their major metabolites in urine is presented. This method can be used for quantitation of amitriptyline, nortriptyline, imipramine, desipramine, doxepin, desmethyldoxepin, and maprotiline in human urine, in addition to the qualitative determination of their hydroxylated metabolites. This method is suitable for confirmation of drug abuse in health care professionals and overdose cases where the identity of the abused cyclic antidepressant may not be known. Samples are spiked with internal standard and hydrolyzed with beta-glucuronidase from Escherichia coli. Hydrolysis is found to be essential to the extraction procedure as the tertiary cyclic antidepressants are found to be extensively conjugated in urine. The secondary cyclic antidepressants, on the contrary, are found to be minimally conjugated. Drugs are extracted from alkalinized urine into solvent and derivatized with MSTFA/ammonium iodide/ethanethiol reagent. This reagent produces more stable derivatives compared to reagents previously employed. Gas chromatographic (GC)-mass spectrometric analysis is performed in electron ionization mode by selective ion monitoring, using hydrogen as a carrier gas, a short narrow bore GC capillary column, and fast temperature program, allowing for a rapid analytical cycle. While maintaining specificity for these drugs, concentrations in human urine ranging from 50 to 20,000 ng/mL can be measured with intraday and interday precisions, expressed as variation coefficient, of less than 2.8% for all analytes.     

Identification of basic drugs in urine by dual fused silica capillary column GC

A method for analyzing urine for the presence of basic drugs and their metabolites using two fused silica capillary columns is described along with operating conditions and column characteristics. Urine extracts were injected into a gas chromatograph equipped with nitrogen phosphorous detectors (GC/NPD) and two capillary columns, housed in a single injection port. The injected material was simultaneously chromatographed in each column. Identification of unknowns was done using relative retention times.     

Urinary metabolites of French maritime pine bark extract in humans

After oral administration of 5.28 g and 1.06 g of French maritime pine bark extract to a human volunteer, metabolites of some of the components of the extract could be detected. Ferulic acid and taxifolin, conjugated as glucuronide/sulphate, were excreted within 18 h. The peak urinary excretion was observed approximately 2-3 h after intake. Recovery of ferulic acid in urine was 36-43% and 7-8% for taxifolin. Two further metabolites could be identified as delta-(3,4-dihydroxy-phenyl)-gamma-valerolactone and delta-(3-methoxy-4-hydroxyphenyl)-gamma-valerolactone conjugated with glucuronic acid/sulphate. These metabolites could also be detected after intake of 960 mg of a procyanidin fraction of French maritime pine bark extract. Thus, it was shown that procyanidins are metabolised by humans. Both metabolites show maximal urinary excretion 8-12 h after intake and are excreted within 28-34 h.     

人尿中卡鲁睾酮的代谢产物研究

使用GC/MS方法对人尿中卡鲁睾酮(calusterone)的代谢情况进行了研究。尿样经XAD-2树脂柱吸附、酶水解、乙醚萃取及三甲基硅烷衍生化处理后,使用毛细管柱进行GC/MS分析,鉴定了7种代谢物,从而推导出卡鲁睾酮在人体中的代谢模式。     

Endocrine effects of cannabis in male rats

Male Wistar rats were administered either synthetic Δ⁹-tetrahydrocannabinol (Δ⁹-THC) or Mexican cannabis extract at doses of 1, 5, 10, 25, and 50 mg of Δ⁹-THC/kg of body weight. Steroid concentrations in urine and blood were measured using glass capillary gas chromatography and individual metabolites were identified by gas chromatography/mass spectrometry. Plasma corticosterone and its metabolite were elevated in a dose-response fashion up to 25 mg/kg. While testosterone is unaltered by Δ⁹-THC, except at 50 mg/kg, ⊙ther metabolites with possible relation to androgen metabolism were elevated. Measurable amounts of estrogens were produced by male rats given the drugs. Additional alterations were seen in the concentrations of conjugated steroids.     

七种常见巴比妥和导眠能的气液色谱法及其从脏器肝和尿中的检出

本文用浓度1.5%的OV-17和SE-52填充柱研究了巴比妥、异戊巴比妥、戊巴比妥、速可眠、硫喷妥、苯巴比妥、美导眠(Heptabarbitone)等七种常见巴比妥和导眠能的气液色谱分离检定条件并实际应用于从人尿,人肝、狗肝、兔肝中检出某些巴比妥类药物。同分异构体如异戊巴比妥和戊巴比妥用本法可以得到较明显的分离。一次色谱过程最多只要20分钟,故为一个快速、高效、灵敏的方法。     

Detection of alprazolam (Xanax) and its metabolites in urine using dual capillary column, dual nitrogen detector gas chromatography

Alprazolam (Xanax) is a fairly new, yet very popular benzodiazepine tranquilizer. In 1985, it was 6th on a nationwide list of drugs mentioned in emergency room drug poisonings. A procedure was developed that allows alprazolam and its main urinary metabolites, alpha-hydroxyalprazolam and 3-hydroxymethyl-5-methyltriazolyl chlorobenzophenone, to be detected in urine specimens. A dual capillary column, dual nitrogen detector gas chromatographic system was used for reliable identification. Improved chromatographic performance was obtained by acetylating the metabolites. Method characteristics such as linearity, reproducibility, limit of detection, and recovery were determined. The method was tested by assaying urine specimens from hospitalized patients who had been ingesting alprazolam. In most cases, alpha-hydroxyalprazolam was found in the highest concentration and separated best from endogenous urine substances. A single dose concentration-time study was performed, and the time course of alprazolam and metabolite concentrations over 48 hours was determined.