柽柳花挥发性成分研究

目的:定性分析柽柳花中的挥发性成分。方法:采用固相微萃取技术提取柽柳花的挥发性成分,采用气相色谱-质谱联用技术结合保留指数法鉴定其成分。结果:从柽柳花的挥发油中共鉴定出36个化合物,其中含量最高的是十五烷(9.80%),其次为6,10,14-三甲基-2-十五烷酮(7.61%)、5,6-二氢-6-戊基-2H-吡喃-2-酮(6.83%)、十六烷(6.25%)和二氢猕猴桃内酯(5.13%)。结论:本研究可为进一步开发利用柽柳资源提供科学依据。     

多枝柽柳挥发性成分分析

目的:定性分析多枝柽柳的挥发性成分。方法:采用固相微萃取技术提取多枝柽柳的挥发性成分,采用气相色谱-质谱联用结合保留指数法鉴定。结果:共分离出34个成分,鉴定了其中的25个,用峰面积归一化法测定了其相对质量分数,占挥发性成分总峰面积的89.50%。其主要成分是十五烷(16.83%)、壬醛(12.45%)、十六烷(8.20%)、十四烷(8.08%)和己醛(7.37%)。多枝柽柳挥发性成分主要含有烃、醛、酮和醇4类化合物,其中烃类的含量最高,为37.11%;其后依次为醛类(占27.56%)、酮类(占8.89%)、醇类(8.04%)。结论:本研究可为进一步开发利用红柳资源提供科学依据。     

海桐种子醇提物中挥发性成分的GC-MS分析及抗内毒素活性测定

目的：研究海桐种子乙醇总提取物(简称EESPTA)的挥发性成分及相对含量,考察其抗内毒素活性。方法：以水蒸气蒸馏法提取EESPTA的挥发性成分,用气-质联用技术分析鉴定,并用峰面积归一化法测定各成分相对含量,采用终点基质显色法鲎实验检测其对细菌内毒素的清除效果,考察其抗内毒素活性。结果：气-质联用技术共检测鉴定出32个色谱峰,占该挥发性成分总量的99.82% 。在EESPTA的挥发性成分中,1R,4S,7S,11R-2,2,4,8-四甲基三环[5.3.1.0(4,11)]十一碳-8-烯含量高达54.78%,其它含量较高的成分有2-亚甲基-胆甾烷-3-醇(7.27%)、蛇麻烷-1,6-二烯-3-醇(6.23 %)、4-甲基-5-癸醇(4.11%)、绿花白千层醇(3. 86%)、别香橙烯(3. 80%)、反式-2,3-二甲基丙烯酸(3. 50%)、二氢-噻喃-3,5-二醇-四氢-4-甲基-4-氮-二乙酸乙酯(2. 04 %)等成分。结论：EESPTA具有较明显的清除细菌内毒素作用,并呈浓度依赖关系。为进一步开发利用海桐药用价值提供了科学依据。     

甘草挥发性成分GC-MS分析

目的对甘草挥发性成分进行研究。方法用水蒸汽蒸馏法提取甘草挥发性成分并采用气相色谱-质谱技术对其进行分析分离、鉴定。结果初步分离出40余个峰,鉴定出32种成分,用峰面积归一化法确定其相对含量。在被测物质中,醇、酚、酯类化合物有2,6-双(1,1-二甲基乙基)-4-甲基苯酚(20.16%)、邻苯二甲酸二甲酯(6.82%)等8种;酸类化合物有正十六酸(8.33%)、正十八酸(4.68%)等8种;烃类化合物有正十九烷(4.71%)、正十八炕(4.16%)、正十七烷(4.02%)等14种;还有2个酮类化合物。结论通过对甘草挥发性成分的研究,为甘草资源的进一步开发利用提供实验依据。     

细叶桉果实CO_2超临界流体萃取物化学成分的GC-MS分析

目的:分析经CO2超临界流体萃取(SFE-CO2)技术提取的广西细叶桉果实的化学成分。方法:采用SFE-CO2法从细叶桉果实中提取化学成分,气相色谱-质谱联用法对其进行分析,并用峰面积归一化法确定各化学成分的相对百分含量。结果:细叶桉果实的SFE-CO2提取物共鉴定出34种化合物,占色谱峰总面积的80.26%。其化学组分主要是二十九烷(10.36%)、1,1′-(1,2-乙基)二十氢萘(8.20%)、3(-1-甲酰基-3,4-亚甲二氧基苯基)苯甲酸甲酯(5.04%)、二十七烷(5.04%)、十五烷(4.84%)、甲氧基肉桂酸乙酯(4.33%)、9-甲基十九烷(4.24%)等。结论:SFE-CO2法可用于细叶桉果实中化学成分的提取,简便、快捷、效率较高。本研究可为细叶桉果实的进一步开发利用提供科学依据。     

翅萼石斛脂溶性成分的GC-MS研究

目的:分析翅萼石斛脂溶性化学成分。方法:采用石油醚超声提取法提取翅萼石斛的脂溶性成分,通过气相色谱-质谱联用法分析和鉴定化学成分(并用面积归一化法获得各化合物的相对质量分数)。结果:共鉴定出34种化合物,相对含量占总含量的71.859%,主要成分包括棕榈酸甲酯(3.913%)、邻苯二甲酸二丁酯(37.174%)、硬脂酸甲酯(2.526%)、十七烷(1.446%)、9-辛基十七烷(1.133%)、四十四烷(1.078%)、二十五烷(6.158%)、邻苯二甲酸二异辛酯(4.757%)、二十一烷(3.767%)。结论:为进一步确定翅萼石斛的化学成分和研究利用提供了一定的参考。     

顶空固相微萃取气质联用分析天山翠雀花中挥发性成分

目的 分析天山翠雀花挥发性成分.方法 采用顶空固相微萃取气质联用(HS-SPME-GC-MS)方法对天山翠雀花挥发性成分进行提取并鉴定,以色谱峰面积归一化法计算各成分的相对百分含量.结果 天上翠雀花中鉴定的挥发性成分共31个.其主要成分为6,10,14-三甲基-2-十五烷酮(8.57%)、(E)-2-庚烯醛(8.25%)、苯乙醇(8.19%)、(E,E)-2,4-庚二烯醛(5.65%)和正辛醇(5.51%)等.结论 天山翠雀花的主要挥发性成分为醛类、酮类和醇类化合物.     

顶空固相微萃取-气质联用技术分析川芎酒炙前后的挥发性成分

目的:比较川芎生品和酒炙品挥发性成分的差异,为川芎的药理活性研究及临床应用提供参考。方法:采用顶空固相微萃取-气质联用技术分析川芎酒炙前后的挥发性成分,并运用面积归一化法计算各成分的相对百分含量。结果:从川芎生品中分离出28个成分,鉴定出24个成分,占总挥发性成分的99.70%,含量较高的分别为2-甲基-2,3-二氢-1H-茚-2-醇(20.06%)、α-芹子烯(17.97%)及4-乙基-壬烯-5-炔(9.24%)。从川芎酒炙品中分离出21个成分,鉴定出18个成分,占总挥发性成分的89.74%,含量最高的为4-乙基-壬烯-5-炔(12.97%),其次为4-蒈烯(11.74%)和α-芹子烯(10.79%);与生品相比,有效镇痛成分α-蒎烯、β-榄香烯含量有所增加。结论:川芎酒炙前后挥发性成分及相对百分含量存在一定差异,酒炙后挥发性成分相对减少,但有镇痛作用的成分含量增加,镇痛效果优于生品。     

GC-MS法检测球花石斛花中挥发性成分

目的研究球花石斛花中挥发性的化学成分。方法采用水回流法从球花石斛花中提取挥发性成分,并用气相色谱—质谱(GC-MS)联用技术,对球花石斛花中的挥发性成分进行了测定。结果共鉴定出22种化学成分,其中含量较高的主要有亚油酸(51.82%)、亚麻酸(10.056%)、棕榈酸(9.282%)、硬脂酸(4.579%)、8-羟基-4,7-二甲基香豆素(4.727%)、6,7-二甲氧基香豆素(3.083%)、二十三烷(4.490%)等。结论该文首次采用气相色谱-质谱(GC-MS)联用技术对球花石斛花挥发性成分进行提取研究。     

细叶桉叶超临界CO_2萃取挥发油的GC-MS分析

目的:分析经超临界CO(2SFE-CO2)萃取的细叶桉叶挥发油的化学成分。方法:采用SFE-CO2法从细叶桉叶中提取挥发油,用气相色谱-质谱联用技术对其化学成分进行分析,并用归一化法确定各化学成分的相对百分含量。结果:细叶桉叶挥发油中共提取、鉴定出28种化合物,占色谱峰总面积的88.13%。其挥发性组分主要是桉油精(33.99%)、冰片(8.88%)、α-蒎烯(5.39%)、石竹烯(4.51%)、(+)-4-蒈烯(4.19%)等。结论:本研究可为细叶桉叶的进一步开发利用提供科学依据。     

Analysis of volatile oil in Rhizoma ligustici chuanxiong-Radix paeoniae rubra by gas chromatography-mass spectrometry and chemometric resolution

AIM: To analyze the volatile chemical components of the herbal pair Rhizoma Ligustici chuanxiong-Radix paeoniae rubra (RLC-RPR) and compare them with those of each of the herbs alone. METHODS: Gas chromatography-mass spectrometry (GC-MS), a chemometric resolution technique using the heuristic evolving latent projections (HELP) method, and the overall volume integration method were used. RESULTS: In total, 52, 38, and 61 volatile chemical components in RLC, RPR, and RLC-RPR essential oils were determined, respectively, accounting for 95.14%, 95.19%, and 89.68% of the total contents of essential oil of RLC, RPR, and RLC-RPR, respectively. The main volatile chemical components were butyldienephthalide (20.65%) and ligustilide (50.15%) for RLC; and n-hexadecanoic acid (20.18%), [Z,Z]9,12-octadecadienoic acid (30.11%), 2-hydroxy-benzaldehyde (17.08%) for RPR, and butyldienephthalide (14.80%), and ligustilide (38.91%) for RLC-RPR. The main volatile chemical components of RLC-RPR were almost the same as those of RLC, but the relative amounts were altered. CONCLUSION: The number of volatile chemical components in RLC-RPR was almost equal to the sum of the number in the 2 constituent herbs, but the relative amounts were altered. Furthermore, an acid-base reaction takes place during the process of decocting the herbs. The data gathered in this study may be helpful for understanding the synergistic nature of this herb pair in traditional Chinese medicine.     

Metabolism of lenampicillin hydrochloride. II. Metabolism of promoiety

The in vitro and in vivo metabolism of promoiety in lenampicillin hydrochloride (LAPC) were investigated in rats and dogs. After incubation of LAPC with intestinal or liver preparations and blood of rat, diacetyl, acetoin and 2,3-butanediol were identified as metabolites of LAPC. The main metabolite in peripheral plasma was 2,3-butanediol after oral administration of LAPC in rats and dogs. On the other hand, high levels of acetoin were found out in portal plasma for early period after dosing of LAPC. These results suggested that the biotransformation of promoiety in LAPC to acetoin carried out mainly in intestinal tissues, but acetoin was converted to 2,3-butanediol in liver. Acetoin and 2,3-butanediol were also excreted in urine, but their urinary excretion were very low, and the combined excretion were accounting for about 9% of dose up to 48 hours after dosing in rats and less than 1% in dogs, respectively. The major metabolic pathways of promoiety in LAPC were postulated as below. (Formula: see text).     

Possibility of diacetyl and related compounds as the 4-carbon compound necessary for the formation of riboflavin in Ashbya gossypii

The effects of various compounds (0.5%) involved in the butanediol and the glycolytic pathways on riboflavin formation in whole cells of Ashbya gossypii at rest were examined. The addition of acetate, glycerol and diacetyl inhibited riboflavin formation, while the addition of acetoin had no effect on it, and the addition of ethanol, 2,3-butanediol, pyruvic acid and glucose accelerated it. The relation of diacetyl and acetoin to riboflavin formation during resting cell incubation in the presence of 0.5% ethanol and various concentrations of 2,3-butanediol was examined. The results quantitatively revealed a precursor-product relation between riboflavin formation and the formation of diacetyl and acetoin. The results obtained provide evidence that a high flavinogenic agent, ethanol, was converted to acetaldehyde, pyruvic acid, acetoin and diacetyl in this order, that a week flavinogenic agent, 2,3-butanediol, was transferred to diacetyl through acetoin, and that the diacetyl produced can be utilized as the 4-carbon compound for riboflavin formation in the flavinogenic mold, Ashbya gossypii. It remains obscure whether diacetyl is enzymatically involved in riboflavin formation.     

藏药大花红景天挥发油化学成分的气相色谱-质谱分析

目的　对大花红景天挥发油的化学成分进行分析。方法　采用水蒸气蒸馏法提取大花红景天挥发油,并通过气相色谱—质谱(GC -MS)联用技术,对其中的化学成分进行分析鉴定。结果　通过计算机检索,鉴定了其中的4 5个化合物,占挥发油色谱峰总面积的96 .6 1 %。主要成分为正辛醇(2 0 .31 %)、牛儿醇(1 2 .86 %)、2 -甲基- 3-丁烯- 2 -醇(1 2 .0 7%)、3-甲基- 2 -丁烯醇(6 .6 9%)、十六酸(6 .4 3%)、亚油酸(5 .73%)、环癸烷(4.0 5 %)等。检出成分占挥发油总量的96 .5 6 %。结论　所用方法为大花红景天的合理利用提供了科学依据。     

兴安白芷的挥发油成分分析

目的:研究兴安白芷(Angelica dahurica Benth.et Hook.f.ex Franch.et Sav.的干燥根)挥发油的化学成分,并分析其与祁白芷挥发油成分之间的异同。方法:采用水蒸气蒸馏法提取挥发油,采用毛细管气相色谱-质谱联用技术分析其挥发油成分。结果:从兴安白芷挥发油中检出244个色谱峰,鉴定了76个化合物,占挥发油总量的86.13%。挥发油主要成分为十四烷醇(tetradecanol,19.43%)、α-柠檬烯(α-limonene,15.25%)、3-蒈烯(3-carene,10.94%)、正十二烷醇(1-dodecanol,5.74%)和1R-α-蒎烯(1R-α-pinene,3.85%)。结论:兴安白芷和祁白芷共有成分有38个,占兴安白芷挥发油总量的34.54%,其倍半萜及其衍生物类成分的数目和含量要远远低于祁白芷。     

Quantitative high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry analysis of the adenine-guanine cross-links of 1,2,3,4-diepoxybutane in tissues of butadiene-exposed B6C3F1 mice

1,3-Butadiene (BD) is an important industrial chemical used in the manufacture of rubber and plastics as well as an environmental pollutant present in automobile exhaust and cigarette smoke. It is classified as a known human carcinogen based on the epidemiological evidence in occupationally exposed workers and its ability to induce tumors in laboratory animals. BD is metabolically activated to several reactive species, including 1,2,3,4-diepoxybutane (DEB), which is hypothesized to be the ultimate carcinogenic species due to its bifunctional electrophilic nature and its ability to form DNA-DNA and DNA-protein cross-links. While 1,4- bis-(guan-7-yl)-2,3,-butanediol ( bis-N7G-BD) is the only type of DEB-specific DNA adduct previously quantified in vivo, four regioisomeric guanine-adenine (G-A) cross-links have been observed in vitro: 1-(guan-7-yl)-4-(aden-1-yl)-2,3-butanediol (N7G-N1A-BD), 1-(guan-7-yl)-4-(aden-3-yl)-2,3-butanediol (N7G-N3A-BD), 1-(guan-7-yl)-4-(aden-7-yl)-2,3-butanediol (N7G-N7A-BD), and 1-(guan-7-yl)-4-(aden-6-yl)-2,3-butanediol (N7G-N (6)A-BD) ( Park ( 2004) Chem. Res. Toxicol. 17, 1638- 1651 ). The goal of the present work was to develop an isotope dilution HPLC-positive mode electrospray ionization-tandem mass spectrometry (HPLC-ESI (+)-MS/MS) method for the quantitative analysis of G-A DEB cross-links in DNA extracted from BD-exposed laboratory animals. In our approach, G-A butanediol conjugates are released from the DNA backbone by thermal or mild acid hydrolysis. Following solid-phase extraction, samples are subjected to capillary HPLC-ESI (+)-MS/MS analysis with (15)N 3, (13)C 1-labeled internal standards. The detection limit of our current method is 0.6-1.5 adducts per 10 (8) normal nucleotides. The new method was validated by spiking G-A cross-link standards (10 fmol each) into control mouse DNA (0.1 mg), followed by sample processing and HPLC-ESI (+)-MS/MS analysis. The accuracy and precision were calculated as 105 +/- 17% for N7G-N3A-BD, 102 +/- 25% for N7G-N7A-BD, and 79 +/- 11% for N7G-N (6)A-BD. The regioisomeric G-A DEB adducts were formed in a concentration-dependent manner in DEB-treated calf thymus DNA, with N7G-N1A-BD found in the highest amounts. Under physiological conditions, N7G-N1A-BD underwent Dimroth rearrangement to N7G-N (6)A-BD ( t 1/2 = 114 h), while hydrolytic deamination of N7G-N1A-BD to the corresponding hypoxanthine lesion was insignificant. We found that for in vivo samples, a greater sensitivity could be achieved if N7G-N1A-BD adducts were converted to the corresponding N7G-N (6)A-BD lesions by forced Dimroth rearrangement. Liver DNA extracted from female B6C3F1 mice that underwent inhalation exposure to 625 ppm BD for 2 weeks contained 3.1 +/- 0.6 N7G-N1A-BD adducts per 10 (8) nucleotides ( n = 5) (quantified as N7G-N (6)A-BD following base-induced Dimroth rearrangement), while the amounts of N7G-N3A-BD and N7G-N7A-BD were below the detection limit of our method. None of the G-A cross-links was present in control animals. The formation of N7G-N1A-BD cross-links may contribute to the induction of AT base pair mutations following exposure to BD. Quantitative methods presented here may be used not only for studies of biological significance in animal models but potentially to predict risk associated with human exposure to BD.     

The Measurement of D,L-2,3-Butanediol in Controls and Patients with Alcoholic Cirrhosis

Plasma D,L-2,3-butanediol was measured in 53 controls and 50 patients with alcoholic cirrhosis, none of whom had measurable amounts of blood ethanol. Thirteen of 50 samples from patients with alcoholic cirrhosis had measurable D,L-2,3-butanediol. (range < 5-154 uM). In one patient with alcoholic cirrhosis who had been abstinent from ethanol for over 5 years plasma levels of D,L-2,3-butanediol ranged between 154 and 211 uM over a one-year period. Only one of the 53 control subjects had detectable levels of D,L-2,3-butanediol. Although it has previously been reported that 2,3-butanediol is present in alcoholics consuming distilled spirits (Runstein et al. (1983) Lancet ii, 534), this is the first report of the persistent presence of these compounds in alcoholics in the absence of ethanol. Clearly in abstinent alcoholics the presence of 2,3-butanediol is not due to the ingestion of undistilled spirits nor is it likely to arise directly from the metabolic products of ethanol. The presence of D,L-2,3-butanediol in patients with alcoholic cirrhosis and its absence in control subjects suggests that this compound may be a marker of some forms of alcoholism.     

Alkyldiol antidotes to ethylene glycol toxicity in mice.

A series of alkyldiols were compared to ethanol or pyrazole as antidotes in ethylene glycol toxicity. Mouse liver alcohol dehydrogenase oxidized ethanol and a series of alkyldiols. The K_m values in millimoles per liter determined from the assays were 0.4 with ethanol, 53 with ethylene glycol, 14 with propylene glycol, 5.4 with 1,3-propanediol, 3.8 with 1,2-butanediol, 1.5 with 1,3-butanediol, 0.5 with 1,4-butanediol, 56 with 2,3-butanediol, 0.23 with 1,5-pentanediol, and 0.031 with 1,6-hexanediol. These data indicated that ethanol and the alkyldiols, with the exception of 2,3-butanediol, had higher affinities for mouse liver alcohol dehydrogenase than ethylene glycol. Propylene glycol (27.2 mmol/kg), 1,2-butanediol (11.2 mmol/kg), and 1,3-butanediol (22.3 mmol/kg) were the only alkyldiols found to protect mice. Acute and delayed toxicity and hexobarbital sleeping time studies indicated that the alkyldiols which protected the mice were, in general, the least toxic and least hypnotic of the alkyldiols. Therapeutic ratios found by dividing the 144 hr LD50 of an antidote by the dose which produced the maximum antidotal effect were 3.17 for ethanol, 2.56 for pyrazole, 6.16 for propylene glycol, 4.15 for 1.2-butanediol, and 5.11 for 1,3-butanediol. These data suggest that the alkyldiol antidotes are effective and may be safter than either ethanol or pyrazole.     

Mutagenesis of the supF gene by stereoisomers of 1,2,3,4-diepoxybutane

1,2,3,4-diepoxybutane (DEB) is a key metabolite of the important industrial chemical and environmental contaminant, 1,3-butadiene (BD). Although all three optical isomers of DEB, S,S-, R,R-, and meso-DEB, are produced by metabolic processing of BD, S,S-DEB exhibits the most potent genotoxicity and cytotoxicity, followed by R,R- and then meso-DEB. Our previous studies suggested that the observed differences between the biological effects of DEB optical isomers may be structural in their origin. Although S,S- and R,R-DEB produced mainly 1,3-interstrand 1,4-bis-(guan-7-yl)-2,3-butanediol (bis-N7G-BD) cross-links, meso-diepoxide induced equal numbers of intrastrand and interstrand bis-N7G-BD lesions. In the present study, the mutagenicity of the three DEB stereoisomers in the supF gene was investigated. We found that S,S-DEB was the most potent mutagen. Interestingly, mutation specificity and mutant spectra were strongly dependent on DEB stereochemistry. Although A:T to T:A transversions were the major form of mutation observed following treatment with each of the three stereoisomers (35-40%), S,S-DEB induced higher numbers of G:C to A:T transitions, whereas R,R-DEB treatment resulted in a greater frequency of G:C to T:A transversions. Our results are consistent with the stereospecific induction of promutagenic nucleobase adducts other than G-G cross-links by DEB stereoisomers.