2种检测灯盏花素血药浓度方法的比较

目的：建立测定Beagle犬血浆中灯盏花素浓度的反相高效液相色谱法和液相-质谱联用法,并将其进行多参数的两两比较。方法：采用液-液萃取法处理血清,反相高效液相色谱法测定,流动相为甲醇-水（pH3．0）=42：58,EclipseXDB-C18为固定相;将同样的样品用液相-质谱法开展平行检测;将所测得的数据做两两对比,采用SPSS统计软件进行分析。结果：2种方法测定的数据具有良好的相关性（r=0．982,P〉0．05）;最低检测限前者为0．05μg／mL,后者为0．01μg／mL,反相高效液相色谱法的最低检测限和灵敏度不及液相-质谱联用法。结论：反相高效液相色谱法可用于灯盏花素毒代动力学研究,与液相-质谱联用法检测结果无显著差异,且费用较低,不失为-种低成本且行之有效的检测方法。     

怀牛膝挥发油成分分析

用气相色谱-质谱联用法定性,气相色谱法定量,首次分析了牛膝(Achgranthesbidentata B1.)干燥根的挥发油的化学成分.共鉴定了45个化合物.特征性成分为2,6-二甲基吡嗪,2-甲氧基-3-异丙基吡嗪和2-甲氧基-3-异丁基吡嗪.     

羌活挥发油成分分析

从羌活、宽叶羌活的根茎及根中提取了挥发油,用气相色谱-质谱联用法分析挥发油的化学成分,共鉴定了136个成分(羌活78个成分、宽叶羌活58个成分),用气相色谱法测定了挥发油各成分的相对百分含量,其鉴定率分别达到94.90％和91.41％。     

连翘挥发油成分分析

从连翘果实中提取了挥发油,用气相色谱-质谱联用法分析其挥发油的化学成分,鉴定出β-蒎烯、香桧烯、α-蒎烯等56个化合物,并用气相色谱测定了挥发油中各成分的相对含量,其鉴定率达93.37％。     

一种被毛孢(Hirsutella sp.)培养液中自由基清除剂的分析、分离和制备

[目的]在一次对虫生真菌代谢物进行大规模的清除自由基活性物质筛选中,发现一种被毛孢(Hirsutella sp.)菌株RCEF0881发酵液中存在有较强的清除自由基活性物质.本研究目的是初步搞清这些活性成分的具体组成,并制备出一定量的纯品用于进一步的结构鉴定.[方法]用有机溶剂法提取活性成分;用二苯基苦基苯肼自由基(DPPH)酶标仪法和薄层色谱法进行活性测定;用高分辨液质联用方法进行活性成分初步分析和鉴定;用反相制备色谱法制备活性组分.[结果]提取实验结果表明具清除自由基活性的物质能较好地被乙酸乙酯提取出来;液相色谱-质谱-活性测定分析表明提取物中活性组分的可能分子式分别为C7H6O4、C8H8O3和C12H14N2O.结合色谱特性、紫外光谱特征、质谱碎片和数据库查询可初步推断它们分别为二羟基苯甲酸、羟基甲基苯甲酸和生物碱类物质,但具体结构还有待于进一步确认.从高效液相色谱和质谱离子流的峰面积可知上述3种活性物质中C12H14N2O的含量最高.本研究成功地用反相制备色谱制备出该天然活性组分的纯品.该3种清除自由基活性物质都是首次发现存在于虫生真菌的代谢物中.     

LC-MS/MS法测定人血浆中伊伐布雷定浓度及药动学

目的：建立人血浆中伊伐布雷定的液相色谱-质谱-质谱联用测定方法,研究健康人体药代动力学。方法：以地西泮为内标物,采用液相色谱-质谱-质谱联用法,电喷雾电离源选择性正离子峰检测。测30名健康志愿者单剂量口服盐酸伊伐布雷定片的体内血药浓度,获得药动学参数。结果：伊伐布雷定在0.101-101 ng·mL-1浓度范围内呈良好的线性关系（r=0.998）,最低检测浓度为0.101 ng·mL-1。高、中、低浓度的方法提取回收率分别为93.2%、86.6%、87.5%,日内、日间精密度RSD均小于15%。结论：LC-MS/MS方法灵敏度高,专属性强,准确,简便,适用于盐酸伊伐布雷定片的人体药代动力学研究。     

SDE—GC—MS分析红雪茶和白雪茶的挥发性成分

采用同时蒸馏萃取法(SDE)分别从红雪茶和白雪茶中提取它们的挥发性成分,用气相色谱-质谱(GC-MS)联用法定性,峰面积归一化法定量,并和相同处理过程的普通绿茶青山绿水相比较.实验结果表明:红雪茶和白雪茶在组成及含量上有很多相似之处,而和绿茶差异较大.     

湿地蒿挥发油成分研究

目的:分析湿地蒿的化学成分. 方法:采用水蒸气蒸馏法提取,运用毛细管气相色谱-质谱联用法对湿地蒿挥发性化学成分进行了分析,用气相色谱面积归一化法测定了各成分的相对百分含量. 结果:经毛细管色谱分离了38个峰,并鉴定出峰所对应的化合物.其主要化学成分为7,11-二甲基-1,6,10-十二碳三烯(56.20%);IR-α-蒎烯(18.63%);3-(苯二甲酰亚氨甲基)-苯甲酸(4.8%);1-甲基-4-(1-甲基乙基)-1,4-环己二烯(3.46%);6,6-二甲基-2-亚甲基-[3,1,1]二环庚烷(1.41%);庚烷(1.28%)等.     

一株蛹拟青霉(Paecilomyces militaris )深层发酵产物中抗肿瘤活性物质分析

摘要： 【目的】初步搞清一株蛹拟青霉（Paecilomyces militaris ）菌株RCEF0927在发酵罐发酵条件下发酵液的抗中国仓鼠卵巢瘤（CHO）细胞活性及活性成分的具体组成。【方法】用刃天青（Resazurin）法测定样品对CHO细胞的抑制率;用高效液相色谱-高分辨质谱和活性测定联用的方法进行活性成分分析和鉴定。【结果】活性测定结果表明菌株RCEF0927经发酵罐发酵的发酵液具有较强的抗CHO细胞活性;提取实验结果表明抗肿瘤活性物质能较好地被乙酸乙酯提取出来;液相色谱-质谱-活性测定分析表明     

小花琉璃草精油成分的研究

用气相色谱-质谱联用法分析了小花琉璃草精油的化学成分,鉴定了茴香脑、爱草醚、小茴香酮、对-甲氧基-苯甲醚等64个化合物,并用气相色谱测定了精油中各成分的相对含量。     

A sensitive method for quantitation of gamma-hydroxybutyric acid and gamma-butyrolactone in brain by electron capture gas chromatography.

A new and sensitive method for the quantitation of γ-hydroxybutyric acid (GHB) and its lactone precursor γ-butyrolactone (GBL), has been developed and successfully utilized to determine the endogenous content of these compounds in a single rat brain. The method involves conversion of endogenous GHB into GBL and extracting the GBL with CHCl₃. The concentrated CHCl₃ extract is treated with BF₃ methanol reagent to produce methyl γ-hydroxybutyrate. Introduction of electron capturing groups was accomplished by further reacting the methyl γ-hydroxybutyrate with heptafluorobutyric anhydride in the presence of pyridine. Prior to quantitation by electron capture gas chromatography, the sample was cleaned up by thin layer chromatography (tlc) using a preabsorbent plate which removed many extraneous peaks as well as CHCl₃ used as the solvent. The effciency of the procedure was evaluated by carrying [1-¹⁴C]GBL through the derivatization. This indicated that about 15% of the starting labeled GBL was converted to the final electron capturing product. δ-Valerolactone was used as an internal standard.     

Chromatographic separation of 2,3-benzodiazepines

A review of chromatographic methods for the determination of 2,3-benzodiazepines (2,3-BZs) is presented. The determinations are performed to investigate the presence of potential impurities in drug substances and to study their pharmacokinetic profile in biological samples, either in animals or in humans. Several methods dealt with a pretreatment of samples, i.e., liquid–liquid extraction by using a variety of solvents, solid-phase extraction, direct injection of specimens into the chromatographic apparatus. Different chromatographic techniques have been used. High-performance liquid chromatography allows optimal sensitivity and specificity by using ultraviolet or diode array detection methods. Gas chromatography-mass spectrometry and gas chromatography with nitrogen-phosphorous or electron-capture detectors have been also reported. Suitable methods for the separation of enantiomers of 2,3-BZs have been described. Thin-layer chromatography has been shown to be capable to isolate analytes from biological samples as urine or faeces. The reported chromatographic techniques are currently applied to define the metabolic pathways of 2,3-BZs in experimental and clinical studies.     

真菌生物量指示剂麦角固醇的分离及测定方法

麦角固醇作为真菌细胞膜的重要组成成分,结构稳定,可作为真菌生长的指示物质。综述了表征真菌生物量的麦角固醇的分离及测定方法,其中麦角固醇的萃取方法有传统的皂化回流法、快速物理萃取、超声波萃取、超临界流体萃取等,测定方法有高效液相色谱法、气相色谱-质谱法、液相色谱-质谱法、薄层色谱法等。并对这些方法的应用及在堆肥过程中运用麦角固醇估计真菌生物量的可行性进行了展望。     

Basic and Neutral Compounds in the Cooked Odor from Antarctic Krill

The cooked odor concentrate from precooked krill was obtained by a simultaneous distillation and extraction system. The resulting odor concentrate was separated into basic, carbonyl and carbonyl-free fractions. Each fraction was analyzed by gas chromatography and gas chromatography-mass spectrometry. Fifty seven compounds, including 3 pyridines, 10 pyrazines, 6 thiazoles, 3 dihydro-4H-1,3,5-dithiazines, 11 aldehydes, 10 ketones, 4 alcohols, 6 hydrocarbons and 4 other compounds were identified. Twenty two of these compounds were newly found as the odor components of krill. The low molecular aldehydes, which are known to be a part of the precursors of the secondary formation of the cooked odor, were also investigated by thin layer chromatography. Ethanal, propanal and butanal were newly detected.     

Measurement of oxidatively induced DNA damage and its repair,by mass spectrometric techniques

Abstract

Oxidatively induced damage caused by free radicals and other DNA-damaging agents generate a plethora of products in the DNA of living organisms. There is mounting evidence for the involvement of this type of damage in the etiology of numerous diseases including carcinogenesis. For a thorough understanding of the mechanisms, cellular repair, and biological consequences of DNA damage, accurate measurement of resulting products must be achieved. There are various analytical techniques, with their own advantages and drawbacks, which can be used for this purpose. Mass spectrometric techniques with isotope dilution, which include gas chromatography (GC) and liquid chromatography (LC), provide structural elucidation of products and ascertain accurate quantification, which are absolutely necessary for reliable measurement. Both gas chromatography-mass spectrometry (GC-MS) or liquid chromatography-mass spectrometry (LC-MS), in single or tandem versions, have been used for the measurement of numerous DNA products such as sugar and base lesions, 8,5’-cyclopurine-2’-deoxynucleosides, base-base tandem lesions, and DNA-protein crosslinks, in vitro and in vivo. This article reviews these techniques and their applications in the measurement of oxidatively induced DNA damage and its repair.     

Separation methods used for Scutellaria baicalensis active components

Scutellaria baicalensis Georgi is one of the most widely used traditional Chinese herbal medicines. Its roots have been used for anti-inflammation, anticancer, antiviral and antibacterial infections of the respiratory and the gastrointestinal tract, cleaning away heat, moistening aridity, purging fire, detoxifying toxicosis, reducing the total cholesterol level and decreasing blood pressures. Baicalin, baicalein, wogonin and oroxylin A are its main active components. This review provides an overview of various separation, detection, and identification techniques employed for the quantitative and qualitative determination of these active components. Applications of high-performance liquid chromatography, high-speed counter-current chromatography, thin layer chromatography, capillary electrophoresis, and micellar electrokinetic capillary chromatography to the separation and determination of these active components are described. Examples of identification of these active components and their metabolites in complex matrices by high-performance liquid chromatography-mass spectrometry and gas chromatography-mass spectrometry are also presented. The advantages and limitations of these separation and identification methods are assessed and discussed.     

Apical dominance and the levels of indole acetic acid in Phaseolus lateral buds

Combined gas chromatography-mass spectrometry procedures have been used to establish that the indole acetic acid levels of lateral buds from Phaseolus seedlings rise following removal of the shoot apex.Abbreviations GC gas chromatograph - GC-MS combined gas liquid chromatography mass spectrometry - bis-TMS bis-trimethylsilyl - IAA indole acetic acid - MPM multiple-peak monitoring - MS mass spectrometer - GLC gas liquid chromatography - TLC thin-layer chromatography     

Detection of gamma-hydroxybutyrate in striatal microdialysates following peripheral 1,4-butanediol administration in rats

The illicit use and abuse of 1,4-butanediol (1,4-BD) results from its presumed conversion to gamma-hydroxybutyrate (GHB) and subsequent pharmacological effects via action on GABA-B and GHB-specific receptors. Using in vivo microdialysis we measured the appearance of GHB in the striata of rats after peripheral 1,4-BD administration. We developed and utilized an HPLC-UV (215 nm) detection of GHB that yielded a limit of quantification (S/N=10) of 2.0 micro g/mL (40 ng/injection) and a limit of detection (S/N=3) of 0.75 micro g/mL (15 ng/injection). GHB appeared in the striatal microdialysates within 20 min after intraperitoneal (i.p.) administration of varying doses of 1,4-BD. GHB concentrations reached dose-dependent maxima 80-100 min post-1,4-BD administration, with peak values of 10.6+/-2.9, 25.3+/-3.4 and 48.1+/-7.1 micro g/mL (mean+/-S.E.M.), corresponding to 1,4-BD doses of 250, 500 and 750 mg/kg, respectively. The conversion of 1,4-BD to GHB was completely prevented by the alcohol dehydrogenase inhibitor 4-methylpyrazole (4MP), administered prior to 1,4-BD, as evidenced by the failure of GHB to appear in the striatal microdialysates. Sleep times in animals were similarly correlated with GHB concentrations in the microdialysates.     

Use of atmospheric pressure ionization mass spectrometry in enantioselective liquid chromatography

Recent advances in mass spectrometry have rendered it an attractive and versatile tool in industrial and academic research laboratories. As a part of this rapid growth, a considerable body of literature has been devoted to the application of mass spectrometry in studies involving enantioselectivity, molecular recognition, and supramolecular chemistry. In concert with separation techniques such as capillary electrophoresis and liquid chromatography, mass spectrometry allows rapid characterization of a large array of molecules in complex mixtures. A majority of these findings have been made possible by the introduction of 'soft-ionization' techniques such as electrospray ionization interface. Other techniques such as atmospheric pressure chemical ionization mass spectrometry have been widely used as a rugged interface for quantitative liquid chromatography-mass spectrometry. Herein, we present a brief overview of the above techniques accompanied with several examples of enantioselective capillary electrophoresis- and liquid chromatography-mass spectrometry in drug discovery and development. Although the emphasis of this article is on quantitative enantiomeric chromatography-mass spectrometry, we envisage that similar strategies are adaptable in qualitative studies.     

Determination of gamma-hydroxybutyric acid in biological fluids by using capillary electrophoresis with indirect detection

gamma-Hydroxybutyric acid (GHB) is a central nervous system (CNS) depressant and hypnotic which, in recent times, has shown an increasing abuse either as recreational drug (due to its euphoric effects and ability to reduce inhibitions) or as doping agent (enhancer of muscle growth). Analogues of GHB, namely gamma-butyrolactone (GBL) and 1,4-butanediol (1,4-BD), share its biological activity and are rapidly converted in vivo into GHB. At present, GHB and analogues are placed in the Schedules of Controlled Substances. Numerous intoxications in GHB abusers have been reported with depressive effects, seizures, coma and possibly death. The purpose of the present work was the development of a rapid analytical method based on capillary zone electrophoresis for the direct determination of GHB in human urine and serum at potentially toxic concentrations. Analytical conditions were as follows. Capillary: length 40 cm (to detector), 75 microm i.d.; buffer: 5.0 mM Na(2)HPO(4), 15 mM sodium barbital adjusted to pH 12 with 1.0 M NaOH; voltage: 25 kV at 23 degrees C; indirect UV detection at 214 nm; injection by application of 0.5 psi for 5 s. alpha-Hydroxyisobutyric acid was used as internal standard (IS). Sample pretreatment was limited to 1:8 dilution. Under these conditions, the sensitivity was approximately 3.0 microg/ml (signal-to-noise ratio >3). Calibration curves prepared in water, urine and serum were linear over concentration ranges 25-500 microg/ml with R(2)>/=0.998. Analytical precision was fairly good with R.S.D.<0.60% (including intraday and day-to-day tests). Quantitative precision in both intraday and day-to-day experiments was also very satisfactory with R.S.D.相似文献