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.

Quantitative analysis of trace levels of β-ionone in water by liquid-liquidphase extraction-gas chromatography-mass spectrometry(LLE-GC-MS)

A simple and rapid technique based on liquid-liquid extraction coupled to gas chromatography-mass spectrometric detection(LLE-GC-MS) was developed for analysis of taste and odour compound β-ionone in water. Instrument parameters including programmed oven temperature, injection temperature and ion source temperature were evaluated and optimized. Effects of extraction time, ionic strength and p H on the detection efficiency were investigated and optimum conditions were 8 min of extraction time, without Na Cl addition at p H=9. Good linearity(R2=0.9997) was obtained when the linear range was 10-500 μg/L. The recoveries of β-ionone in ultrapure water and tap water samples were 88%-95% and 110%-114%, respectively. The relative standard deviations(RSD) were less than 10%. The method detection limit(MDL) and rejection quality level(RQL) were achieved at1.98 μg/L and 6.53 μg/L, respectively. LLE-GC-MS was demonstrated to be a rapid and convenient method for the determination ofβ-ionone in water samples.

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.

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。

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。

GC-MS Analysis of Essential Oil Constituents from Rhizome and Root of Notopterygium forbesii

Aim To analyse the chemical constituents of the essential oil extracted from the rhizome and root of Notopterygium forbesii Boiss. and provide scientific basis for quality control. Methods The total essential oil was extracted by water-steam distillation and separated by capillary gas chromatography (GC). The components were determined by normalization method, and identified by GC-MS. Results GC-MS exhibited 217 peaks and 100 compounds were identified, accounting for 78.3% of the total essential oil. Conclu...

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 Analysis of Essential Oil Constituents from Rhizome and Root of Notopterygium incisum

Aim To analyse the chemical constituents of the essential oil extracted from the rhizome and root of Notopterygium incisum Ting ex H.T. Chang, providing scientific basis for quality control. Methods The total essential oil was extracted by water-steam distillation and separated by capillary gas chromatography （GC）. The components were determined by normalization method, and identified by GC-MS. Results GC-MS exhibited 242 peaks and 83 compounds were identified, accounting for 75.77% of the total essential oil. Conclusion In the total essential oil of the rhizome and root of N. incisum, monoterpenes and sesquiterpenes accounted for 13.63% and 67.93%, respectively, in which （ 1S）-β-pinene （ 1.67% ）, 3-carene （ 1.05% ）, limonene （ 1.22% ）, and 1S-endo-bornyl acetate （ 1.68% ） as the monoterpenes and its derivatives, and （ ＋ ） -β-elemene （6.78%）, sativene （1.54%）, α-caryophyllene （2.64%）, germacrene D （1.67%）, eudesma-4 （ 14 ）, ll-diene （2.36%）, α-selinene （2.42%）, δ-cadinene （ 1.55% ）, 3,7,11-trimethyl-2,6,10-dodecatrien-1-ol （1.03%）, （ ＋ ）-elemol （5.18%）, （-）-spathulenol （1.40%）, guaiol （3.81%）, dehydroxy-isocalamendiol （ 1.06% ）, γ-eudesmol （ 1.05% ）, α-eudesmol （7.97%）, bulnesol （3.09%）, and carotol （2. 30% ） as the sesquiterpenes and its derivatives were main components. In addition, isopropyl transcinnamate was the maximum compound （ 11.3% ） of the total essential oil.

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.

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。

Rapid and simultaneous determination of ten off-flavor compounds in water by headspace solid phase microextraction and gas chromatography-mass spectrometry

A simple and sensitive analytical procedure for the determination of multi-component compounds in water samples was developed and optimized using the headspace solid-phase microextraction(HSSPME) coupled with gas chromatography-mass spectrometry(GC-MS). Ten off-flavor compounds, including geosmin(GSM), 2-methylisoborneol(2-MIB), 2-isopropyl-3-methoxypyrazine(IPMP), 2-isobutyl-3-methoxypyrazine(IBMP), β-ionone, trans-2,cis-6-nonadienal(NDE), 2,3,4-trichloroanisole(2,3,4-TCA), 2,3,6-trichroloanisole(2,3,6-TCA), 2,4,6-trichloroanisole(2,4,6-TCA), and 2,4,6-tribromoanisole(2,4,6-TBA) were used as the target analytes. The optimization of extraction parameters including fibers types, extraction time, extraction temperature, stirring rate, sample volume, and ionic strength was carried out through the univariate approach. Ten off-flavor compounds were quantified within 50 min under the optimal conditions. Calibration curves with good linearity(r^2=0.990-0.998) were obtained in the range 1.0/2.0-100 ng/L, while the limits of detection for all compounds were lower than or close to the odor threshold concentration. Furthermore, the proposed method was applied to analyzing and determining the off-flavor compounds in real water samples from water-treatment plants.

Simultaneous Determination of 8 Pesticide Residues in Green Tea Based on Gas Chromatography-mass Spectrometry

To improve pesticide residues detection efficiency in tea, simultaneous de- termination of eight pesticide residues in green tea was developed based on gas chromatography-mass spectrometry （GC-MS）. The results showed that, - detected by the GC-MS under following conditions： acetonitrile as extraction and elution solvent, activated carbon and PSA tandem column as the stationary phase, elution volume of 12 ml the relationship between peak area and concentration of each residue （ametryn in the range of 0-100 pg/L, napropamide in the range of 0-10 000 gg/L, other pesticides in the range of 0-1 000 tJg/L） were linearly related, and their corre- lation coefficients were all greater than 0.999. The recovery rate the pesticides added to tea sample at legal concentration limits ranged from 73.6% to 116.8%, and the relative standard deviation from 1.47% to 15.58%. The new method we de- veloped is sensitive, specific and anti-interference, and thus provides test basis for the development of pesticide matrix reference materials in tea.