This work is to analyse volatile compounds of four plants-Hedychium coronarium Koenig,Hedychium flavum Roxb,Hedychium sinoaureum Stapf,Hedychium forrestii.SDE-GC-MS was set up to analyse volatile compounds of four plants in hedychium,and their differences were discussed.105 volatile compounds were isolated and identified from the four plants,mainly are terpenoids and their oxygenated compounds.There are lots of active ingredients in the four plants,and their volatile compounds are similar,but the content of components in Hedychium flavum Roxb is different from the others.

A new phenolic compounds, gramphenol A, together, with three known phenols (2-4), were isolated from the whole plant of Arundina gramnifolia. The structure of compounds 1-4 was elucidated by spectroscopic methods including extensive D-1 and (2D) NMR techniques. The anti-tobacco mosaic virus (anti-TMV) activities were evaluated for Compounds 1-4. The results reveal that compound 1 exhibits modest anti-tobacco mosaic virus activities.

We analysed volatile compounds in Matthiola incana,and evaluated the effect of its cigarette flavoring.Simultaneous distillation and extraction(SDE)-GC-TOFMS technology was set up to analyse volatile compounds in Matthiola incana,area normalization method was used to calculate each component relative content,then the oil was added into cigarette to proceed sensory evaluation.66 volatile compounds are isolated and identified from Matthiola incana,the main ones are 2-β-Pinene(13.28%),3-Carene(10.16%),(-)-Isoledene(4.80%),β-Bourbonene(4.53%),Spathulenol(3.39%)and β-Cadinene(3.29%) etc.Evaluation results show that:moderate concentration of volatile oil can improve the overall coordination of cigarette,reduce thrill of oral cavity and nasal cavity,reduce mixed gas,make aftertaste sweet and fresh,etc.There are lots of volatile components in Matthiola incana,mainly are terpenoids and their oxygen derivatives,in which lots of are aromatic substances and active ingredients.They are foundations of new approaches/new methods for the exploitation and utilization of Matthiola incana.

OBJECTIVE:To analyze volatile compounds of Elsholtzia communis.METHODS:Simultaneous distillation and extraction(SDE)-GC-MS and Head-space injection(HS)-GC-MS technology were set up to analyze volatile compounds in E.communis,and the influence of steaming temperature and solid-liquid ratio on the essential oil yield of E.communis were discussed.RESULTS:121 volatile compounds were isolated and identified from E.communis,and the main components were citral,acetic acid,etc.Besides,the yield of essential oil was 2.40% on the condition that steaming time was 5 hours,solid-liquid ratio was 1:30(m/V),which better than others.CONCLUSION:The information about volatile compounds in E.communis obtained by SD from literature reports,SDE,HS have different focus.SDE is more plentiful than obtained by SD or HS analysis.We can get a better representation system for GC-MS fingerprints of volatile compounds in E.communis when combine these methods together.

本文采用同时蒸馏萃取法分别对莲雾新老叶片和柚子新老叶片4个样品进行提取,提取物通过高分辨飞行时间质谱结合多维数理统计的方法进行分析,对比研究了两种植物不同生理期叶片的挥发性成分差异.结果表明:莲雾叶提取物与柚子叶提取物的挥发性成分由于植物品种的不同具有较大区别,而其中莲雾新老叶片挥发性成分之间的差异较柚子新老叶片显著,另外还对莲雾新老叶片提取物与柚子新老叶片的提取物的部分协方差系数大于0.1的离子碎片进行定性分析.根据得到的结果,确定了这两种香原料的最佳采摘收获期,对这两种植物作为香原料应用具有十分重要的指导意义.

Objective To analyse volatile compounds in Kaempferia rotunda.Methods Simultaneous distillation and extraction(SDE)-GC-MS technology was set up to analyse volatile compounds in Kaempferia rotunda.Results 51 volatile compounds are isolated and identified from Kaempferia rotunda,the main ones are α-pinene(6.83%),camphene(13.00%),β-pinene(18.97%),camphor(5.80%),linalool oxides(5.11%)etc.Conclusion There are lots of volatile components in Kaempferia rotunda,mainly are terpenoids and their oxygen derivatives,in which lots of are aromatic substances and active ingredients.

The research advances in Plumeria rubra in recent years were systematically discussed from its volatile components and pharmacological research,providing references for improving the clinical efficacies and safety of P.rubra.

By the methods of field observation and artificial pollination,this paper studied the characteristics of pollination biology and breeding system of endangered species Craigia yunnanensis in the fragmented habitats of Fadou distribution area,Xichou County of Yunnan Province,Southwest China.Each cyme of the C.yunnanensis had 2-9 hermaphroditic flowers,and the lifespan of a single hermaphroditic flower was approximately 3-4 days.There existed certain temporal isolation(dichogamy) and spatial isolation(herkogamy) between the pistils and stamens of each hermaphroditic flower.The outcrossing index(OCI) was 4,and the ratio of pollen to ovule(P/O) was 1381±53.The most frequent and effective pollinator was Chrysomyia megacephala.The fruiting rate of geitonogamous pollination was rather low,and thus,the breeding system of C.yunnanensis was mainly belonged to outcrossing,with partial self-compatibility,and the pollinator insects were essential.Both the fruit-setting ratio and the seed-bearing ratio under natural conditions were low as 56.67%±3.85% and 6.26%±0.75%,respectively,whereas artificial xenogamous pollination could significantly promote the fruit-setting and seed-bearing ratios(P 0.01).In the fragmented habitats,the pollinators were lesser,and the pollination efficiency was lower,suggesting that habitat fragmentation affected the early stage reproduction process of C.yunnanensis plants.

A new norlignan, nicotnorlignan C (1), together with four known norlignans (2-5) were isolated from the roots and sterns of Nicotiana tabacum. Tie structures of compounds 1-5 were elucidated on the basis of extensive NMR and MS means. The anti-tobacco mosaic virus I activity of 1-5 was evaluated. All the compounds showed modest anti-tobacco mosaic virus activity.

[Objective] To study the methods for extracting volatile components from Schizonepeta tenuifolia Briq.[Method] The volatile components were extracted from the S.tenuifolia by simultaneous distillation extraction,backward flow,program raise of temperature microwave extraction and headspace.Then,GC-TOFMS was used to analyse their components and relative content.Besides,effects of different extracting technologies on volatile components were also compared.[Result] 60,27,38 and 34 volatile components were identified from S.tenuifolia extracts prepared by simultaneous distillation,backward flow,program raise of temperature microwave extraction,and headspace,respectively.Both components and relative content of volatile components were notably different in extracts prepared by different method.Moreover,estragole was the main component of the above S.tenuifolia extracts that accounted for 34.90%,39.90%,39.90%,and 84.82%,respectively.[Conclusion] The simultaneous distillation extraction is better than others,which could be used for analysing volatile components in S.tenuifolia.

[Objective] To analyze volatile compounds of Alpinia officinarum Hance. [Method] Simultaneous distillation and extraction （SDE）-GC-MS technology was set up to analyze the volatile compounds of A.officinarum. [Result] A total of 72 volatile compounds were isolated and identified from A.officinarum, the main ones were 1, 8-cineole （38.54%）, α-terpinenyl acetate （6.55%）, torreyol （7.74%）, isolongifolene （3.64%）, ledene （3.93%） etc. [Conclusion] The information about volatile compounds of A.officinarum obtained by SDE is different from those obtained by steam distillation or headspace analysis, and more plentiful than them. We can get a better representation system for the volatile compounds of A.officinarum when combine these methods together.

Phenol in mainstream of cigarette smoke was trapped in 35 mL of dilute acetic acid solution(1+99 by vol.).The solution obtained was diluted to 50 mL,from which an aliquot of 2.0 mL was taken for the rapid HPLC analysis.The ZORBAX Stable Bound column(2.1 mm×50 mm,1.8 μm) was used for the rapid separation,and mixtures of acetonitrile(containing 1% by volume of acetic acid) and dil.acetic acid solution(1+99) mixed in various ratios were used as mobile phase in the gradient elution.Fluorescence detection with the wavelengths of 272 nm(λex) and 310 nm(λem) was adopted in the determination.Only 5.0 min were required for a determination.The repeatability and reproducibility of the method were tested,giving values of RSD′s(n=7) 2.8% and 4.6% respectively.Test for recovery was made by standard addition method at 3 concentration levels,values of recovery found were in the range of 95%-103%.

In order to study the effects of processing condition on the change of chemical components in tobacco,different conditions of storing were simulated in laboratory and their effects on the main chemical components in different grades of tobacco leaves were orthogonally experimented.The results showed that when the significance level α is to 0.05,the significance change chemical components include total sugars,reducing sugars,total nitrogen,amina acid,non-volatile acid,petroleum ether extract,polyphenol.When the significance level α = 0.05 and 0.1,the significance change related parameter include environment temperature,environment humidity,storing time.

Content of the six heavy meta1 elements in main-stream smoke was determined by atomic absorption spectrometry and atomic fluorescence spectrometry in order to study impacts of different characters of cigarette paper and tip paper,as well as percentage of delivery amounts of heavy meta1 elements to tar.Results indicated that the amounts of heavy metal elements in main stream smoke decreased with the decrease of tar.However,the decreasing amplitudes of these heavy metal elements and tar were different.It was showed that cigarette paper with higher air permeability(when air permeability lower than 70CU),tipping paper with electrostatic perforation,tipping paper perforated near lip end were helpful for reducing the amounts of heavy meta1 elements in main stream smoke while maintaining certain tar amount.

A gas chromatography-mass spectrometry method for the determination of polyphenols (chlorogenic acid, rutin and scopoletin) in tobacco samples was studied. The polyphenols were extracted from the samples by ultrasonic extraction and a 99:1 mixture of N,O-bis(trimethylsilyl)trifluoroacetamide and trimethylchlorosilane was used for derivatization. With GC-MS detection in single-ion-monitoring mode, the main polyphenols (chlorogenic acid, rutin and scopoletin) were analyzed quantitatively. The limit of detections (S/N = 3) were below 50 ng/mL, the relative standard deviations (RSD) were below 3.2 % (n = 7) and the recoveries were in the range of 92-106 %.

Crotonaldehyde in mainstream of cigarette smoke was trapped and derivatized simultaneously on a piece of cambridge filter(on which 2 mL of 0.075 mol·L-1 2,4-dinitrophenylhydrazine-acetonitrile solution,or abbreviated as DNPH solution,were dropped homogeneously and dried in a desiccator,ready for use) by smoking 2 cigarettes with a smoking machine.A mixed solution of pyridine and acetonitrile(2+98) was used to extract the derivatized product of 2,4-dinitrophenylhydrazone from the filter into the extraction solvent.An aliquot of the extract was used for HPLC analysis.Rapid separation of crotonaldehyde in the extract was attained within 5.5 min by using ZORBAX Stable Bound C18(2.1 mm×50 mm,1.8 μm) column and by using mixtures of acetonitrile(A) and water(B) of different ratios for gradient elution.DAD at the wavelength of 365 nm was adopted in the determination.Detection limit(3S/N) found for the method was 8.0 μg·L-1.Tests for recovery were made at 3 concentration levels(0.05,0.10,0.2 mg),and results of recovery found were in the range of 96%-101%.Repeatability and reproducibility were also tested and the values of RSD′s(n=7) founs were 2.2% and 2.9% respectively.

[Objective] The aim was to discuss the effect of using rapid column high performance liquid chromatography to determine vanillin in chocolate.[Method] The rapid column high performance liquid chromatography was used to determine vanillin in chocolate.[Result] 40 ml 40% methanol were selected to extract vanillin from chocolate by ultrasonic for 10 min,then solid phrase extraction was applied for pre-separation.The vanillin was separated with ZORBAX Stable Bound(4.6×50 mm,1.8 μm) C18 as stationary phase and methanol-water(35∶65) as mobile phase at flow-rate of 10 ml/min,and the detector was UV photodiode array detector.Under the chromatographic conditions,vanillin could reach baseline separation in 1.0 min.The sample standard recoveries were 98%-103% and the relative standard deviations were 0.46%-0.58%.The separation time could be shortened above 85% compared with conventional chromatograph.[Conclusion] The method was convenient and rapid,and the result was reliable,which provided method for rapid determination of vanillin in chocolate to some extent.

The determination of imidacloprid in tobacco with high performance liquid chromatography was studied. The imidacloprid was extracted from the sample with ethyl acetate, and purified be liquid extraction with 5% Sodium chloride solution and dichloromethane, respectively. The imidacloprid was separated on a ZORBAX Stable Bound (2.1×50 mm, 1.8 m m) column with acetonitrile and 0.01 mol/L ammonium acetate solution as mobile phase at a flow-rate of 1.0 mL/min. The imidacloprid can be separated completely with in 2.5 min. This method was applied to the determination of imidacloprid in tobacco. The relative standard derivation of intra-day variations was 3.6%, and the relative standard derivation of inter-day variations was 4.8%. The standard recoveries were ranged from 88-96%.

[Objective]The study aimed to establish the rapid analysis method to determine water in tobacco essence by Karl Fischer method. [Method] After automatic pre-titration and calibration with cassette reagent, the moisture contents in 4 kinds of tobacco essence were titrated by cassette reagent, and the moisture content in environment was titrated in order to eliminate background interference. At the same time, the recovery rate was calculated according to measured quantity before adding standard, adding standard and measured quantity after adding standard. The relative standard deviation was calculated according to the determination results from 6 parallel determinations on tobacco essence. [Result] Analysis results of determining the moisture contents in tobacco essence by using Karl Fischer method were satisfactory, with the relative standard deviation at 1.65%-2.54% and the recovery rate of 93.46%-106.15%. The determination on the moisture contents in tobacco essence by using Karl Fischer method showed that the moisture contents in 4 kinds of tobacco essence had great difference, which was in 1.49%-5.74% and the result was satisfactory. [Conclusion] Using Karl Fischer method to determine water in tobacco essence was sensitive, accurate, well repeatable, and provided a reference for determining water in tobacco essence.

A new ion chromatographic method is developed for the determination of ammonia in mainstream cigarette smoke. The ammonia in mainstream cigarette smoke was collected by diluted sulfuric acid with an absorption vessel designed in our laboratory. The interference of tar and nicotinamide was separated by solid phase extraction with graphitized carbon black cartridge. The ammonia was determined by ion chromatography, and the whole procedure of the determination could be completed in 12 min. The detection limit was 0.005 m g/mL and the RSD 2.8%. The recoveries of fortified blanks and fortified matrix were 96.5%-101.5% and95%-102%, respectively. This method has been applied to the determination of ammonia in mainstream cigarette smoke of 10 kinds of cigarettes of China with satisfactory results. Copyright CJI.