人体液中喷布洛尔及其代谢物的GC/MS分析

用气相色谱一质谱联用(GC-MSD)系统分析方法检出了人尿中喷布洛尔的6个羟化代谢物,用Scp-Pak柱提取的方法检出了人血浆中的原型药物。并从分子结构上对此药物的代谢途径进行了研究。尿中提取和血中提取的回收率分别为90.83.%和85.88%,Gc-MSD的检测限为5pg。本方法适用于运动员兴奋剂的系统检查。     

营养补充品中刺激剂的分析测定

介绍营养补充品中刺激剂的毛细管气相色谱和气相色谱质谱联用检测方法.试样采用碱提,液-液分配提取,以HP-5毛细管柱为分离柱,用氮磷检测器测定.实验结果表明:该方法操作简便,分析速度快,结果可靠.添加平均回收率为75.4%～143.1%,相对标准偏差为0.27%～5.5%,检出限为5～40μg/L.     

Method for the Determination of Diphenhydramine in Rabbit Whole Blood by High-Performance Liquid Chromatography (HPLC) with Ultraviolet (UV) Detection in Conjunction with Gas Chromatography (GC) with Mass Selective Detection (MSD)

An HPLC/GC-MSD method for the determination of diphenhydramine in rabbit whole blood has been developed and validated. This method is based on a liquid–liquid extraction and reversed-phase Chromatography with ultraviolet absorbance detection monitored at 258 nm. HPLC eluant fractions containing diphenhydramine and the internal standard, orphenadrine, were collected, reex-tracted, then subjected to GC-MSD analysis. Whole blood was utilized, thereby decreasing the required sample volume and increasing the sensitivity of the assay. Diphenhydramine concentrations can be quantitated over a range of 1 to 1000 ng/ml whole blood.     

羚羊角中脂肪酸类成分的GC-MSD分析

目的：阐明羚羊角中脂肪酸类成分。方法：溶剂法提取脂类成分,经甲酯化,采用气相色谱一质谱．计算机联用技术分离鉴定,归一化法计算相对百分含量。结果：从羚羊角中鉴定出9种脂肪酸类成分,占总脂的85．14％,其中不饱和脂肪酸3种,占17．92％。结论：羚羊角中主要脂肪酸类成分为棕榈酸、硬脂酸、油酸,占80．31％。     

气相色谱-质谱法快速测定面粉中过氧化苯甲酰

目的:建立快速测定面粉中过氧化苯甲酰的定性定量测定方法。方法:采用改进的前处理方法,用气相色谱-气质联用仪进行定性定量分析。结果:过氧化苯甲酰的方法最低检出限为0.5μg/m l,其在2.5~500μg/m l范围内呈线性关系,相关系数大于0.9995,RSD小于5%,回收率为95.8%~102.5%之间。结论:本法灵敏度高,操作简单,稳定性和重复性好,适合测定面粉中过氧化苯甲酰含量的检测。     

Butyl and Phenyl Tin Compounds in Fish and Shellfish on the Korean Market

The degree of organotin contamination was determined in samples of ten species of fish and shellfish that were representative of the Korean fish market. Shellfish and fish samples were collected in the fish markets of eight big cities in Korea (Gangneung, Ulsan, Pusan, Daegu, Guangju, Daejun, Incheon and Seoul). The edible portion of total 160 samples were analyzed for organotin compounds such as monobutltin (MBT), dibutyltin (DBT), tributyltin (TBT), monophenyltin (MPT), diphenyltin (DPT) and TPT (triphenyltin) by GC-MSD SIM mode after propylation and Florisil clean-up. Generally organotin levels of fish were higher than shellfish. The highest concentration of TBT was found in mackerel (average 67.02 ng/g-wet wt.) among fish and shellfish. TBT usually accounted higher percentage than that of MBT and DBT in most samples. However, the average concentration order of PTs in the tested samples was MPT > TPT > DPT except saury.     

冰片和川芎嗪血药浓度的GC－MSD测定法

建立了用气相色谱—质谱检测法同时测定血浆中冰片和川芎嗪血药浓度的方法。冰片和川芎嗪浓度在１０～３００ｎｇ／ｍｌ范围内线性关系良好。冰片和川芎嗪的血中回收率分别为９７．３２％和８７．３７％；最低检测浓度为２ｎｇ／ｍｌ。本方法以樟脑为内标，ＳＩＭ方式检测，定量准确、干扰小，日内及日间的相对标准偏差分别小于４％和７％。并应用本法成功地进行了动物实验和健康人含服速效救心丸后冰片的药代动力学研究。     

气相色谱—质谱法测定血中伪麻黄碱

应用毛细管气相色谱一质量选择检测器(GC-MsD),以麻黄碱为内标,测定血浆中伪麻黄碱浓度。选择离子检测方式(SIM)可避免生物样品中许多杂质干扰,且灵敏度高、准确性好,已成功地用于伪麻黄碱的生物利用度和药代动力学研究。     

刺激剂类药物及代谢物的分离鉴定

报道了41种刺激剂的气相色谱和质谱数据以及人尿中原药和它们的游离型和结合型代谢物的分离和鉴定方法。用分辨率高的毛细管气相色谱分离,以灵敏度高专属性好的氮磷检测器检测志愿者24 h尿样中游离型母体药及代谢物。选择部分时间收集尿样进行直接气质联用分析以及采用三氟醋酰化、三甲基硅烷化和两者并用的衍生化方法鉴定母体药及游离型代谢物。尿样酸水解后,再进行以上选择性衍生化,可测定它们的结合型代谢物。     

香叶天竺葵挥发油的化学成分及抗瘤作用

用高分离效能的交联石英毛细管柱气相色谱法和气相色谱/质量选择检测器分离和鉴定了三种香叶油,并作了对比。结果表明这些香叶油的化学成分极为相似,但某些成分的含量却有明显差别。香茅醇、香叶醇、甲酸香茅酯和乙酸香茅酯均有一定的抗瘤活性。