GC/MS,SIM定性定量分析食品中的苏丹红1号

目的 探讨GC/MS测定苏丹红1号的分析方法.方法 用二氯甲烷和乙腈将苏丹红1号从样品中提取出来,运用GC/MS的Xcalibur分析软件的检索功能.从样品谱图中检索出苏丹红1号,并应用GC/MS快速准确的定量测定苏丹红1号的含量.结果 该方法标准曲线的线性范围1～10.0 pg,检出线0.05 μg/ml,样品加标回收率89.3%～98.3%,平均94.4%.从1件样品中检测出苏丹红1号,含量为0.05 g/kg.结论 该方法简便、快速、灵敏度高、准确可靠.     

混合滥用药物的气相色谱质谱分析

目的 :建立混合滥用药物快速、灵敏检测方法。方法 :采用气相色谱 质谱法 (GC MS)对 11种毒品、药品进行定性定量分析。结果 :苯丙胺类及吗啡在 5 0× 10 - 4- 2 0× 10 - 2 g·ml- 1 范围内线性关系良好 ,检出限分别为 1 0×10 - 4g·ml- 1 和 2 0× 10 - 4g·ml- 1 ;氯胺酮、哌替啶、地西泮、咖啡因、可卡因、马来酸氯苯吡及乙酰替乙氧苯胺线性范围为 5 0× 10 - 6 - 5 0× 10 - 4g·ml- 1 ,检出限为 1 0× 10 - 6 g·ml- 1 和 2 0× 10 - 6 g·ml- 1 。结论 :本方法可用于混合滥用药物组分的快速、准确定性定量分析。     

国产盐酸舍曲林胶囊和片剂的人体药物动力学及生物等效性

目的研究国产盐酸舍曲林胶囊及片剂的相对生物利用度、药物动力学特征及生物等效性.方法采用随机、开放、3×3拉丁方设计实验,18名男性健康受试者分别单剂量口服含舍曲林50 mg的试验片剂、胶囊及参比制剂.采用HPLC-MS/MS/MS法测定给药后不同时间的血药浓度,计算3者的药物动力学参数及评价其生物等效性.结果 18例健康志愿者口服参比制剂和试验制剂舍曲林胶囊及片剂后,参比制剂中舍曲林的主要药物动力学参数cmax为(10.14±3.43)μg·L-1;tmax为(4.44±1.10)h;AUC0～96为(262.82±100.66)μg·h·L-1;t1/2为(29.19±4.91)h.试验制剂片剂中舍曲林的主要药物动力学参数cmax为(10.16±3.22)μg·L-1;tmax为(4.33±1.85)h;AUC0～96为(269.71±107.47)μg·h·L-1;t1/2为(30.99±6.49)h.试验制剂胶囊中舍曲林的主要药物动力学参数cmax为(10.39±3.59)μg·L-1;tmax为(4.94±1.30)h;AUC0～96为(264.45±112.57)μg·h·L-1;t1/2为(29.68±5.25)h.试验制剂片剂和胶囊分别对参比制剂的相对生物利用度F为(103.4%±18.2%)、(99.8%±13.6%).结论经统计学分析,国产试验制剂胶囊剂和片剂与参比制剂具有生物等效性.     

A novel metalloprotease from Vipera lebetina venom induces human endothelial cell apoptosis.

A novel endothelial cell apoptosis inducing metalloprotease (VLAIP) was found in the snake venom of Vipera lebetina. This metalloprotease is a heterodimeric glycoprotein with molecular mass of about 106 kDa. The protease hydrolyzes azocasein, fibrinogen and oxidized insulin B-chain. The enzyme readily hydrolyzes the Aalpha-chain and more slowly Bbeta-chain of fibrinogen. VLAIP does not cleave fibrin. The complete amino acid sequences of the two different monomers of VLAIP are deduced from the nucleotide sequences of cDNAs encoding these proteins. The full-length cDNA sequences of the VLAIP-A and VLAIP-B encode open reading frames of 616 and 614 amino acids that include signal peptide, propeptide and mature metalloproteinase with disintegrin-like and cysteine-rich domains. VLAIP belongs to the metalloprotease/disintegrin family of reprolysins and has high identity with the proteins that induce apoptosis of endothelial cells. Treatment of HUVEC cells with VLAIP induces changes in the attachment of cells to the substrate and causes cell death. We demonstrated that VLAIP inhibits endothelial cell adhesion to extracellular matrix proteins: fibrinogen, fibronectin, vitronectin, collagen I, and collagen IV. The induction of apoptosis by VLAIP was shown by means of a typical DNA fragmentation pattern of apoptotic cells as well as by monitoring phosphatidylserine externalization using annexin V-FITC staining and flow cytometric analysis.     

高效液相色谱法测定红毛五加中绿原酸的含量

目的:采用LC／MS2方法鉴定出中药红毛五加中绿原酸成分,并用高效液相色谱法测定其含量。方法:采用Zorbax SB-C18色谱柱(150 mm×4．6mm,5μm);流动相为乙腈和水(含0．16％甲酸)二元梯度洗脱系统;流速为1．0mL·min-1,检测波长327 nm。质谱条件:Agilent多级离子阱质谱仪:电喷雾化学电离源(ESI);负离子检出模式。结果:绿原酸的线性范围为 10-100 mg·L-1(r=0.9997),加样回收率为99．2％-101．8％;红毛五加中绿原酸的含量为0．58-5．45mg．g-1。结论:本方法灵敏、快速、重现性好,有助于红毛五加质量控制方法的研究。     

超临界流体萃取柴胡果实精油及其化学成分分析

目的:提取柴胡果实精油并分析其化学组成.方法:采用超临界流体革取技术(Supercritical Fluid Extraction,简称SFE)提取柴胡果实的精油,气相色谱-质谱联用仪(GC-MS)分析和鉴定其化学成分.结果:精油的提取率为6.60%(V/W),确定了73个化合物.结论:首次采用超临界革取法从柴胡果实中提取精油,精油的提取率是柴胡根的3倍多,亚油酸、鲸蜡醇乙酸酯、亚油酸乙酯、(-)石竹烯氧化物的相对含量分别为34.85%、16.63%、2.64%、1.81%,植醇、鲸蜡醇乙酸酯、亚油酸乙酯、(-)-石竹烯氧化物为首次从该属植物中发现.     

Supercritical fluid extraction of essential oil from the fruits of Bupleurum chinense DC. and their characterization by GC/MS

IntroductionChaihuhasbeenusedasoneofthecommontraditionalchinesemedicinesandisoftenemployedtotreatcoldswithfever,alternatingchillsandfever,feelingoffullnessandchestoppression,andhypochondriasis[1 ] .Itssaikopaponins ,essentialoilhavebeenwellinvestigated .10ursane typetriterpeneglyco sides,19oleanane typetriterpeneglycosidesfromthefruitsofBupleurumrotundifoliumhavebeenisolated ,inaddition ,ursane typetriterpeneglycosideswereshowedtopossessantiprolifera tiveactivity[2 ] .Toourknowledge ,thechemic…     

Automated solid-phase extraction and two-step derivatisation for simultaneous analysis of basic illicit drugs in serum by GC/MS

A combination of automated solid-phase extraction (SPE) and subsequent two-step derivatisation has been developed for the simultaneous analysis of basic drugs of abuse and cocaine metabolites in serum samples. Substances included in this procedure are morphine, codeine, methadone, cocaine, benzoylecgonine, methylecgonine, amphetamine, methamphetamine, MDMA, MDEA and MDA. SPE with mixed-mode cartridges (RP-C8 and cation-exchange) was fully automated with a Zymark RapidTrace SPE robot. GC/MS analysis was performed after derivatisation with a new two-step reaction by trifluoroacetic anhydride and 2,2,3,3,3-pentafluoropropanol. High recoveries (> 85%) with high reproducibility (CV 1.1-3.8%) were found for all drugs. High correlation coefficients (r > 0.998) were obtained due to the addition of deuterated standards prior to extraction. Experience obtained over 2 years of applying this method to drug analysis in serum is discussed.     

HPLC-MS同时测定4种新型抗抑郁药物的血药浓度

目的:建立一种快速灵敏的同时测定血浆中氟西汀、西酞普兰,帕罗西汀及文拉法辛浓度的 HPLC-MS 方法,监测这4种药物的血药浓度,为临床用药提供依据。方法:以氟伏沙明作为内标,样品碱化后固相萃取,用 MACHEREY-NAGEL C_(18)反相色谱柱(4.6 mm×250 mm,5μm,Germany)进行分离,以乙腈-缓冲盐(30 mmol 醋酸铵和0.6‰甲酸)(65:35)为流动相,柱温40℃,流速0.85 mL·min~(-1)。采用质谱电喷雾电离源(ESI)将样品离子化,选择性离子监测(SIM)准分子离子峰。结果:氟西汀、西酞普兰、帕罗西汀,文拉法辛及内标氟伏沙明在9 min 内完全分离;各物质在5～1000 ng·mL~(-1)时线性关系良好,相关系数均大于0.9964;萃取回收率均大于73.2%;方法回收率均大于95.0%;最低检测浓度:氟西汀0.5 ng·mL~(-1)、西酞普兰0.3 ng·mL~(-1)、帕罗西汀0.3 ng·mL~(-1),文拉法辛0.1 ng·mL~(-1);日内日间变异系数均小于15%。结论:本方法简便快速,灵敏准确,可用于血药浓度的临床监护、中毒分析,药物动力学以及代谢机制的研究。