Super Antibiotics, Part II. Hyperforin, Mass Spectroscopy (MS) and Gas Chromatography-Mass Spectrometry (GC-MS), Evidence of Permeability of the Blood-Testis Barrier (BTB) and the Blood-Brain Barrier (BBB) to Hyperforin

In the first article of this series, we presented some evidence of hyperforin as an antibiotic, antiprotozoal, antiviral, anticancer, and immunomodulatory substance. In the present article, evidence of the permeability of the blood-testis barrier (BTB) and blood-brain barrier (BBB) to hyperforin and its distribution in other organs of the domestic pig (Sus scrofa domesticus) are revealed. Seven-month-old male boars with a body mass of 100 kg were fed a diet containing hyperforin. Organs were surgically removed under anesthesia. Organs were suitable prepared and extracted, and then analyzed using gas chromatography-mass spectrometry with supersonic molecular beams (GC-MS with SMB). The presence of hyperforin was recorded in all organs and body fluids. Special attention was paid to the evaluation of the presence of hyperforin in the brain and testes of experimental animals. The presence of hyperforin in the brain and testes of experimental animals was established by GC-MS with SMB. The results are of interest because penicillin and numerous other antibiotics cannot pass through the BTB or BBB if healthy or non-inflamed, which limits their use in patients with meningitis and gonorrhea. The findings are also of interest in cases of penicillin- and multi-antibiotic-resistant bacterial infections.

Mechanism of Cinnamomum camphora essential oil for analgesia based on gas chromatography-mass spectrometry integrated network pharmacology

This study aims to explore the analgesic ingredients and mechanism of Cinnamomum camphora essential oil(CCEO).The constituents in CCEO were characterized qualitatively by gas chromatography-mass spectrometry.Targets related to active ingredients were collected by PubChem and Swiss Target Prediction.Targets related to pain were screened by TTD and OMIM database,and compound-target network was established by Cytoscape software.Gene ontology(GO)function and Kyoto encyclopedia of genes and genomes(KEGG)pathway enrichment analysis of targets were carried out by DAVID database.Protein-protein interaction(PPI)network was established and analyzed by STRING database.Molecular docking method was used to verify the interaction between main components and relevant core targets.A total of 13 compounds were identified in CCEO,and 58 related targets were predicted.GO function enrichment analysis revealed that the selected targets were mainly involved in biological processes such as chemical synaptic transmission and molecular function such as neurotransmitter receptor activity;24 signal pathways were screened by KEGG pathway enrichment analysis,including neuroactive ligand-receptor interaction,retrograde endocannabinoid signaling and calcium signaling pathway.Docking results showed that the main constituents had certain affinities with the key targets.The active ingredients in CCEO regulated multiple signaling pathways to ameliorate pain through AR,ACHE,ESR1,GABRG2,PTGS2 and PPARγ.

Chemical profiling of bioactive compounds in the methanolic extract of wild leaf and callus of Vitex negundo using gas chromatographymass spectrometry

BACKGROUND The investigation of plant-based therapeutic agents in medicinal plants has revealed their presence in the extracts and provides the vision to formulate novel techniques for drug therapy.Vitex negundo(V.negundo),a perennial herb belonging to the Varbanaceae family,is extensively used in conventional medication.AIM To determine the existence of therapeutic components in leaf and callus extracts from wild V.negundo plants using gas chromatography-mass spectrometry(GCMS).METHODS In this study,we conducted GC-MS on wild plant leaf extracts and correlated the presence of constituents with those in callus extracts.Various growth regulators such as 6-benzylaminopurine(BAP),2,4-dichlorophenoxyacetic acid(2,4-D),α-naphthylacetic acid(NAA),and di-phenylurea(DPU)were added to plant leaves and in-vitro callus and grown on MS medium.RESULTS The results clearly indicated that the addition of BAP(2.0 mg/L),2,4-D(0.2 mg/mL),DPU(2.0 mg/L)and 2,4-D(0.2 mg/mL)in MS medium resulted in rapid callus development.The plant profile of Vitex extracts by GC-MS analysis showed that 24,10,and 14 bioactive constituents were detected in the methanolic extract of leaf,green callus and the methanolic extract of white loose callus,respectively.CONCLUSION Octadecadienoic acid,hexadecanoic acid and methyl ester were the major constituents in the leaf and callus methanolic extract.Octadecadienoic acid was the most common constituent in all samples.The maximum concentration of octadecadienoic acid in leaves,green callus and white loose callus was 21.93%,47.79%and 40.38%,respectively.These findings demonstrate that the concentration of octadecadienoic acid doubles in-vitro compared to in-vivo.In addition to octadecadienoic acid;butyric acid,benzene,1-methoxy-4-(1-propenyl),dospan,tridecanedialdehyde,methylcyclohexenylbutanol,chlorpyrifos,n-secondary terpene diester,anflunine and other important active compounds were also detected.All these components were only available in callus formed in-vitro.This study showed that the callus contained additional botanical characteristics compared with wild plants.Due to the presence of numerous bioactive compounds,the medical use of Vitex for various diseases has been accepted and the plant is considered an important source of therapeutics for research and development.

蒙山名茶蒙顶甘露和蒙山毛峰特征香气成分的GC-MS测定与分析

采用同时蒸馏萃取法和气相色谱质谱（gas chromatography-mass spectrometry ， GC-MS）分析方法系统分析了蒙山茶原产地保护区域内蒙泉、后盐、陇西3个产地及保护区外合江产地蒙顶甘露和蒙山毛峰香气成分的特征与差异.结果表明，在鉴定的63种香气成分中，醇类和醛类占一半以上（59.16％～71.42％）.在蒙顶甘露和蒙山毛峰的香气组分中均以植醇、香叶醇、L-芳樟醇、壬醛和正庚醛这5个成分所占比例较高；保护区内蒙顶甘露和蒙山毛峰最重要的香气特征是植醇和壬醛含量显著高于保护区外，其总量分别占保护区中心内甘露的29.95％和毛峰的40％、保护区外甘露的0％和毛峰的11.27％，同时也是区别于其他名优绿茶的最主要的香气成分.由保护区中心向外延伸，蒙顶甘露和蒙山毛峰的香型有相似的变化规律：由保护区中心的板栗香型经中间的铃兰类鲜爽花香型逐渐过渡至边沿的蜜糖香、花香型.总体上，原产地保护区域内蒙顶甘露和蒙山毛峰的香气品质优于其他非原产地保护区域的蒙顶甘露和蒙山毛峰.

广西八角挥发油的提取研究与GC-MS分析

In this paper,the Illilium verum Hook.f.grow at mountain of Dayao of Jinxiu in Guangxi,Volatile oil was extracted by soxhet method and steam distillation.All the volatile oil was analyzed by GC-MS,the result show the ingredients and rate of product were change greatly,The major chemical constituents were trans-anethole,estragole and anisaldehyde etc.

化妆品中乙醇胺类的GC-MS分析

Gas chromatography-mass spectrometry (GC-MS) method has been developed for the simultaneous determination of monoethanolamine,diethanolamine,triethanolamine in cosmetics.The detected materials were extracted with ethanol by ultrasonic, then were analyzed by GC-FID and GC-MSD.The relative standard deviations (RSD) were 0.76%-3.43%,and recoveries were 85.8%-106.0%. The limit of detection was 0.05%.

大鼠尿液中硝基安定代谢物的GC-MS检验

The metabolites and metabolic passways of nitrazepam in rat were confirmed.Wistar rats were feed a pill of nitrazepam,24 h urine reactions were collected.After β-Glucuronidase hydrolysis of the urine samples,the fractions were extracted by Oasis HLB3cc solid-phase column and analyzed by gas chromatography-mass spectrometry with DB-35 MS column.7-Acetylaminonitrazepam,7-aminonitrazepam and 2-amino-5-nitrophenylphenylmethanone were identified as nitrazepam metabolites.The results suggested that two metabolic passways for nitrazepam may be operative in rat.The first passway leads to the corresponding 7-aminonimetazepam in which the amino group is subsequently acetylated.The second passway is open the parent compounds rings to 2-amino-5-nitrophenylphenylmethanone.Nitrazepam was metabolized quickly in rats and 7-acetylaminonitrazepam were the main metabolites in urine.

藏药甘肃蚤缀脂溶性成分的GC-MS分析

研究藏药甘肃蚤缀的脂溶性成分,进一步揭示该药材的化学成分,为这一传统藏药资源的开发利用提供实验依据。采用95%乙醇回流提取甘肃蚤缀全草,滤液浓缩后用石油醚萃取,得到脂溶性部位,通过气相色谱-质谱联用技术分析其化学成分,结合计算机检索技术及美国国家标准技术研究所(NIST)化合物谱库检索进行鉴定,采用面积归一化法确定其相对含量。从甘肃蚤缀石油醚部位共分离鉴定出25个化合物,相对含量占总含量的91.31%,包括脂肪类、甾体、三萜及芳香化合物等。

HS-SPME-GC-MS技术分析不同加工阶段的甲鱼腥味成分变化

为研究不同加工方式对甲鱼腥味成分的影响,采用HS-SPME-GC-MS技术对甲鱼预煮、卤制、烘烤不同加工阶段的腥味物质进行分析。结果表明,经NIST/Willey质谱数据库检索和文献对照,新鲜甲鱼共检出48种挥发成分,确定36种成分,包括烃类21种、醛类12种、醇类化合物5种、芳香类5种、羧酸类3种、酮类1种、酯类1种。其中以己醛的百分含量最多,为29.1%,有青草味;庚醛占10.69%,具有强烈的油脂氧化味;壬醛占12.58%,提供鱼腥味;占2.02%的对二甲苯有刺激味;占2.36%的1-辛烯-3-醇具有土腥味。认为己醛、壬醛、庚醛、1-辛烯-3-醇等共同形成了甲鱼的腥味。通过预煮、卤制、烘烤等加工工艺后,腥味成分已减少至只能检测出己醛和壬醛,且含量都不超过1%。表明经预煮、卤制、烘烤等加工可以有效控制甲鱼的腥味。

固相萃取及GC-MS分析环境水体中神经性毒剂水解产物

Analysis of nerve agents and their degradation products constitutes an important subject for verifying the compliance to the Chemical Weapons Convention(CWC).In environmental water,the relevant degradation products of nerve agents are usually present at low concentration levels and mixed with a large amount of interferents.In this paper,six different kinds of solid-phase bulk sorbents were respectively investigated to improve the SPE efficiency for nerve agents degradation products from stimulant water samples,in which a large amount of background interferents were spiked.Results showed that the strong anion-exchange sorbent could selectively extract the spiking six target compounds from the matrices and showed a high recovery.

基于GC-FID、HS-SPME-GC-MS与电子鼻技术评价不同水果发酵酒的香气特征

采用气相色谱-氢火焰离子化检测器法(gas chromatography with hydrogen flame ionization detection,GCFID)、顶空固相微萃取-气相色谱-质谱(headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry,HS-SPME-GC-MS)和电子鼻技术分析6种果酒中的挥发性成分,评价果酒风味轮廓特征的差异性。结果表明,GC-FID定量测定樱桃李酒,其中异戊醇、活性戊醇、β-苯乙醇含量最高,乙酸乙酯含量最低;木瓜酒中正丙醇、2,3-丁二醇、癸酸乙酯、乙酸含量最高; 3-羟基-2-丁酮含量在樱桃李酒中最高,山楂酒、甜橙酒中最少。HP-SPME-GC-MS鉴定果酒中挥发性物质94种,其中醇类23种,酯类43种,醛酮类10种,酸类8种,酚类2种,苯环类5种,烷烃类3种。山楂酒、菠萝酒、木瓜酒、甜橙酒、无花果酒和樱桃李酒中香气物质数量分别为34、44、45、45、33、47种。其中山楂酒、木瓜酒和无花果酒中未检出酚类、烷烃类物质。电子鼻对不同果酒香气的区分效果无重叠,W5S传感器区分果酒香气能力最强。比较而言,菠萝酒和樱桃李酒的口感更圆润,香气更愉悦,感官得分最高。

应用GC-MS/MS技术检测水果蔬菜中22种残留农药

To establish a new GC-MS/MS method for quantitative detection of 22 kinds of pesticide in fruit and vegetable including organic phosphorus,carbamate & pyrethrin etc.Working was performed by Xcalibur software with multitask mode.We Carried on qualitative and quantitative analysis to mass spectrum of MS/MS in order to obtained a credible experiment result.This method is sensitive and accurate,it is suitable for determination of multifarious pesticide residues.

GC-MS测定血液中二十八烷醇

Octacosanol in blood was extracted with dichloricmethane.It was derivatized to trimethylsilyl ethers by N,O-Bis(trimethylsilyl) trifluoroacetamide.The compound was determined by gas chromatography-mass spectrometry and selected ion monitoring(SIM).Quantitative analysis was performed by measuring the area and comparing it to a calibration curve.

Determination of 14 Organophosphorus Pesticide Residues in Mutton by Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry(GPC-GC-MS)

[Objectives]This study was conducted to purify mutton samples by gel permeation chromatography(GPC).[Methods]Fourteen organophosphorus pesticide residues in samples were qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry(GC-MS)in selective ion scanning mode(SIM).[Results]The organophosphorus pesticide standard solutions showed good linearity in the mass concentration range of 0.1-10.0μg/ml with correlation coefficients(r)not lower than 0.999,and the detection limits(S=3 N)ranged from 0.01 to 0.05 mg/kg.The average recovery values were in the range of 80.2%-99.7%,with relative standard deviations(RSDs,n=3)in the range of 1.8%-6.3%,at the addition levels of 0.5,1.0 and 2.0 mg/kg.[Conclusions]The method is simple,sensitive and accurate,and can be used for the determination of organophosphorus pesticide residues in mutton.

福建姜黄挥发油化学成分的HS-SPME-GC-MS分析

采用水蒸气蒸馏法提取福建姜黄挥发油,应用顶空固相微萃取进样结合气相色谱-串联质谱联用技术(HS-SPME-GC-MS)分析姜黄挥发油的化学成分。结果表明:姜黄挥发油含有量为7.2%(mL/g),从姜黄挥发油中共分出62个色谱峰,初步鉴定出了其中的51种化学成分,占总挥发油总量的98.41%。在鉴定的化合物中,主要为单萜类化合物和倍半萜类化合物,其中新发现一种主要成分为β-柏木烯,相对含量占比高达26.58%,这可作为福建姜黄挥发油的特征成分和主要品质指标。本研究结果将为福建姜黄植物药材的品质评价提供科学依据。

GC-MS法测定黄酒和食用酒精中的氨基甲酸乙酯

建立应用气相色谱-质谱联用法(gas chromatography-mass spectrometry,GC-MS)快速测定黄酒和食用酒精中氨基甲酸乙酯(ethylcarbamate,EC)的分析方法。以黄酒和食用酒精为研究对象,样品经过碱性硅藻土固相萃取柱净化、浓缩后,用GC-MS进行测定,同位素内标法定量。氨基甲酸乙酯在10~600μg/L线性关系良好,相关系数r^2=0.999 3。加标水平为5、100、250μg/kg 3个浓度条件下,在黄酒中的加标回收率为81.2%~89.5%,每个加标水平测定6次的相对标准偏差(RSD)为3.7%~5.0%;在食用酒精中的加标回收率为91.2%~99.4%,每个加标水平测定6次的RSD为3.1%~4.1%。方法的检出限为1.0μg/kg,方法的定量限为3.0μg/kg。该方法定量准确、操作简便、灵敏度高,适用于黄酒和食用酒精中氨基甲酸乙酯的测定。

Determination of Aromatic Components of Rosa davurica Pall. by Headspace Solid Phase Microextraction Combined with GC-MS

[Objectives] To determine the aromatic components of Rosa davurica Pall. [Methods] 42 kinds of aromatic components were identified from the flowers of R. davurica by headspace solid phase microextraction( HS-SPME) combined with gas chromatography-mass spectrometry( GC-MS). The main compounds were alcohols( 54. 88%) and aldehydes( 19. 55%). [Results] The top five components with the highest relative content were phenylethyl alcohol( 12. 69%),geraniol( 9. 85%),citronellol( 8. 80%),nerol( 7. 84%) and 2-n-pentylfuran( 7. 45%). [Conclusions] Headspace solid phase microextraction( HS-SPME) combined with gas chromatography-mass spectrometry( GC-MS) can provide basis for further development and utilization of R. davurica.

Simultaneous Determination of Hexoestrol, Diethylstilbestrol, Estrone and 17-Beta-estradiol in Feed by Gas Chromatography-mass Spectrometry

A method was developed for the simultaneous determination of four kinds of estrogens （hexoestrol, diethylstilbestrol, estrone, and 17-beta-estradiol） in feed by gas chromatography-mass spectrometry （GC-MS）. After the sample was extracted by ethyl ether and cleaned-up on HLB phase extraction column, four kinds of estrogens were derived and quantified in gas chromatographymass spectrometry. The results showed that the linear detectable ranged from 2.5 ng· mL-1 to 250 ng· mL-1for hexoestrol and from 5 ng· mL-1 to 500 ng· mL-1 for three other estrogens with the correlation coefficients （R2） were no less than 0.990. The recoveries were in the range of 76.34%-96.33% and the relative standard deviation was no more than 22.7%. The limits of quantitation （LOQ） for all analytics were between 10 ug· kg^-1 and 20 ug· kg^-1. The method was accurate and sensitive and could meet the actual requirements for the analyses of feed samples.

Comparative analysis of essential oils found in Rhizomes Curcumae and Radix Curcumae by gas chromatography-mass spectrometry

A comparison of the volatile compounds in Rhizomes Curcumae （Ezhu） and Radix Curcumae （Yujin） was undertaken using gas chromatography mass spectrometi-y （GC-MS）. Ultrasonic extraction and GC-MS methods were developed for the simultaneous determination of five sesquiterpenes, namely, α-pinene, β-elemene, curcumol, germacrone and curdione, in Ezhu and Yunjin. Good linearity （r〉0.999） and high inter-day precision were observed over the investigated concentration ranges. The validated method was successfully used for the simultaneous determination of five sesquiterpenes in Ezhu and Yujin. The quantitative method can be effectively used to evaluate and monitor the quality of Chinese curcuma in clinical use.

Studies on the Components of Essential Oil of <i>Zanthoxylum Armatum</i>by Gc-Ms

The essential oil of Zanthoxylum armatum was extracted through hydro distillation and analyzed by GC-MS. Hydrocarbon fraction (17.35%) of the oil was much lower and oxygenated compounds comprised fairly high portion of essential oil (39.21%). Percentages of monoterpenes and sesquiterpenes found were 47.33% and 10.83% respectively. Oxygenated monoterpenes comprised major profile of chromatogram of essential oil of Zanthoxylum armatum i.e. 37.23% where as monoterpene hydrocarbons were 10.09%. Alcoholic percentage was much higher i.e. 26.76% and 15-hexadecanoloide (6.58%) the only cyclic ester was found in relatively high percentage.