虎乳灵芝栽培品和野生品的脂溶性成分分析

目的比较虎乳灵芝栽培品和野生品脂溶性化学成分的差异。方法采用回流提取法提取虎乳灵芝野生品和栽培品(包括大米和木屑培养)菌核的脂溶性成分,用气相色谱-质谱联用(GC-MS)法分析栽培品和野生品的化学成分,并计算各化学成分的相对百分含量。结果虎乳灵芝大米、木屑栽培品及野生品分别鉴定出11种、10种、14种化合物。主要为烃类化合物,三者共有成分为2,4-二叔丁基苯酚、二十五烷和三十一烷等,并且二十五烷和三十一烷在大米栽培品、木屑栽培品和野生品中相对百分含量分别为15.85%、17.36%、16.43%和12.01%、11.58%、19.29%。三者成分差异表现为:大米栽培品含有麦角甾醇、二十九烷;木屑栽培品含有二十二烷、二十三烷、二十四烷;野生品还含有二十四烷、芥酸酰胺、邻苯二甲酸二丁酯、亚油酸乙酯。结论栽培品和野生品的脂溶性成分中含有2,4-二叔丁基苯酚、二十五烷和三十一烷等相同的化学成分,但又存在明显的差异,可为虎乳灵芝栽培品的质量评价和开发利用提供参考。     

Analysis of endosulfan and its metabolites in rat plasma and selected tissue samples by gas chromatography-mass spectrometry

A method has been developed for the determination of trace levels of alpha-endosulfan, beta-endosulfan, endosulfan sulfate, and endosulfan diol in rat plasma and tissue samples. Endosulfan and its metabolites in the plasma samples were extracted with solid-phase extraction Chromabond-end-capped C18 cartridges and analyzed by a Shimadzu QP-5050A gas chromatograph-mass spectrometer (GCMS) with quadrupole detector in selected-ion-monitoring mode. The analysis of endosulfan and its metabolites in liver and kidney samples involved solvent extraction, Florisil solid-phase-extraction cleanup, and quantitation by GCMS. Recovery experiments for the plasma and tissue samples were conducted over concentration ranges of 10-100 ng mL(-1) and 100-1000 ng mL(-1), respectively. The method was applied to the analysis of trace levels of endosulfan and its metabolites in plasma and tissue samples collected from an animal study. Trace levels of alpha-endosulfan and beta-endosulfan in the ranges of undetectable to 3.11 microg g(-1) and undetectable to 1.19 microg g(-1), respectively, were detected in the kidney samples, whereas trace levels of endosulfan sulfate in the range of 0.02-0.22 microg g(-1) were detected in the liver samples of rats. Neither endosulfan nor its metabolites was detected in any of the plasma samples.     

GC/GCMS analysis of the petroleum ether and dichloromethane extracts of M oringa oleifera roots

ObjectiveTo explore the phytochemical constituents from petroleum ether and dichloromethane extracts of Moringa oleifera (M. oleifera) roots using GC/GC-MS.MethodsA total of 5.11 kg fresh and undried crushed root of M. oleifera were cut into small pieces and extracted with petroleum ether and dichloromethane (20 L each) at room temperature for 2 d. The concentrated extracts were subjected to their GC-MS analysis.ResultsThe GC-MS analysis of the petroleum ether and dichloromethane extracts of M. oleifera roots, which showed promising biological activities, has resulted in the identification 102 compounds. These constituents belong to 15 classes of compounds including hydrocarbons, fatty acids, esters, alcohols, isothiocyanate, thiocyanate, pyrazine, aromatics, alkamides, cyanides, steroids, halocompounds, urea and N-hydroxyimine derivatives, unsaturated alkenamides, alkyne and indole. GC/GC-MS studies on petroleum ether extract of the roots revealed that it contained 39 compounds, belonging to nine classes. Cyclooctasulfur S8 has been isolated as a pure compound from the extract. The major compounds identified from petroleum ether extract were trans-13-docosene (37.9%), nonacosane (32.6%), cycloartenol (28.6%) nonadecanoic acid (13.9%) and cyclooctasulfur S8 (13.9%). Dichloromethane extract of the roots was composed of 63 compounds of which nasimizinol (58.8%) along with oleic acid (46.5%), N-benzyl-N-(7-cyanato heptanamide (38.3%), N-benzyl-N-(1-chlorononyl) amide (30.3%), bis [3-benzyl prop-2-ene]-1-one (19.5%) and N, N-dibenzyl-2-ene pent 1, 5-diamide (11.6%) were the main constituents.ConclusionsThis study helps to predict the formula and structure of active molecules which can be used as drugs. This result also enhances the traditional usage of M. oleifera which possesses a number of bioactive compounds.     

电热蚊香液中拟除虫菊酯成分的气相色谱质谱检测方法

目的建立检测电热蚊香液中多种拟除虫菊酯成分的快速灵敏的分析方法。方法采用气质联用的方法,同时对电热蚊香液中拟除虫菊酯杀虫剂进行定性及定量分析。结果所有5种拟除虫菊酯成分分离良好,标准曲线线性良好,相关系数r0.998,有较好的准确度和精密度,加标回收率在89.1%~102.4%之间,相对标准偏差小于5%。应用该方法对35种电热蚊香液中拟除虫菊酯进行测定,94.3%的有效成分与标识相符,5.7%有效成分品种和含量与商品标识不符。结论实践证明本方法简单、快速、选择性好、灵敏度高,适合日常检测工作的需求。     

An Investigation of Demethylation in the Metabolism of Methoxytryptamine and Methoxytryptophol

Though melatonin is primarily metabolised to 6-hydroxy-melatonin, we have recently shown that it can also be demethylated to form N-acetyl-serotonin. The question therefore arises as to whether demethylation is a general metabolic pathway that can apply to other pineal methoxyindoles. To investigate this possibility we administered deuterated methoxy-tryptophol (dML) and deuterated methoxy-tryptamine (dMT) to rats and analysed the urine for the presence of deuterated methoxyindole acetic acid (dMIAA) and deuterated hydroxyindole acetic acid (dHIAA). The method of analysis was gas chromatography mass spectrometry (GCMS), where the relevant molecular ion and fragment ions were monitored. The results showed that the major metabolite in all cases was dMIAA. There was no evidence to suggest that the compounds had been demethylated to form dHIAA. The study therefore indicates that the demethylation of melatonin is a specific metabolic pathway that does not apply to other methoxyindoles.     

Simultaneous determination of GHB and EtG in hair using GCMS/MS

A gas chromatographic tandem mass spectrometric (GCMS/MS) method for simultaneously determining trace concentrations of gamma-hydroxybutyrate (GHB) and ethyl glucuronide (EtG) in hair has been developed. Multiple reaction monitoring (MRM) was used to detect precursor and product ions of GHB, (233 and 147) and EtG (261 and 143) following anion exchange solid phase extraction and derivatization with N,O-bis[trimethylsilyl]trifluoroacetamide (BSTFA). Deuterated standards of GHB and EtG were used as internal standards. The assay produced excellent linearity (r(2) > 0.99) and sensitivity. The lower limit of quantitation (LLOQ) was 10 pg/mg for EtG assuming a 20 mg hair sample. The method has been used to investigate cases of suspected drug facilitated assault as well as being used to identify heavy alcohol consumption in a group of volunteers.     

A “once a day administration” sustained-release theophylline formulation: Disposition and pharmacokinetics

Summary The pharmacokinetics of a new sustained-release preparation of theophylline (Dilatrane à Action Prolongée capsules filled with homogenous microgranules) has been after its studied administration to 7 healthy volunteers at 8 p.m. in order to achieve therapeutic levels at night and in the morning. In separate trials the test dose of 500 or 600 mg was administered for 7 days, once daily at 8 p.m. Plasma theophylline levels were measured by capillary gas chromatography with a mass specific detector after pentylation, using internal standards labelled with stable isotopes (¹⁵N-1,3 and ¹³C-2 theophylline). The new sustained-release preparation showed a monophasic regular absorption phase with very low interindividual variability. After administration, the plasma level stayed within 80% of the peak levels for 8.5±1.5 h. There was a good correlation between the dose and the steady state plasma level (r=0.9587; p<0.05). This preparation can be chronically administered once daily day at 8 p.m. in order to achieve a therapeutic level during the night and the morning, and to provide sufficient protection during the nycterohemeral period, with a once dose a day schedule.     

Increased breath ethane levels in medicated patients with schizophrenia and bipolar disorder are unrelated to erythrocyte omega-3 fatty acid abundance

Oxidative stress has been reported to be elevated in mental illness. Preliminary evidence suggests this phenomenon can be assessed non-invasively by determining breath levels of the omega-3 polyunsaturated fatty acid (PUFA) oxidation product ethane. This study compares alkane levels in chronic, medicated, patients with schizophrenia or bipolar disorder with those in healthy controls. Both ethane and butane levels were significantly increased in patients with schizophrenia or bipolar disorder, although elevated butane levels were likely due to increased ambient gas concentrations. Ethane levels were not correlated with symptom severity or with erythrocyte omega-3 PUFA levels. Our results support the hypothesis that oxidative stress is elevated in patients with schizophrenia and bipolar disorder leading to increased breath ethane abundance. This does not appear to be caused by increased abundance of omega-3 PUFA, but rather is likely due to enhanced oxidative damage of these lipids. As such, breath hydrocarbon analysis may represent a simple, non-invasive means to monitor the metabolic processes occurring in these disorders.