以芴、苯酚、对甲氧基苯酚和多聚甲醛为原料,采用溶液法合成了直接在芴的苯环结构上进行修饰的2个新型芴基苯并噁嗪单体3-芴基-3,4-二氢-1,3-苯并噁嗪(FBZ-1)和3-芴基-6-甲氧基-3,4-二氢-1,3-苯并噁嗪(FBZ-2).利用FT-IR,1H NMR和13C NMR对其结构进行了表征.采用示差扫描量热法(DSC)研究了2个单体的固化动力学,计算了固化反应活化能,确定了最佳固化温度.通过DSC和热重(TGA)分析了单体及其聚合物的热性能.结果 表明,FBZ-1和FBZ-2呈现出典型的热开环固化特征,放热峰顶温度(5℃·min-1的升温速率)分别为231.2℃,228.7℃,其聚合物初始热分解温度(热失重5％时)达290℃、299℃;850℃时的残炭率(Yc)达到40.9％和36.9％,极限氧指数(LOI)分别是33.86、32.26.

采用顶空固相微萃取-气相色谱-质谱联用技术对L-抗坏血酸-L-半胱氨酸反应体系在不同水分含量下的产物进行鉴定,共鉴定出包括噻吩、硫杂环、噻唑、硫醇、呋喃和硫醚等在内的62种化合物,其中23种噻吩化合物和13种硫杂环化合物为2种主要挥发性产物.结果表明,水分含量对硫杂环类化合物和噻吩类化合物影响明显,而对其他几类挥发性产物的影响不大.随水分含量的增加,硫杂环类产物中3,5-二甲基-1,2,4-三硫环戊烷2种异构体和4,6-二甲基-1,2,3,5-四噻烷3种产物在水分含量为55％时有极大值;2,4,6-三甲基-1,3,5-三噻烷的2种异构体随水分含量的增加而缓慢下降,3-甲基-1,2,4-三噻烷在水分含量为45％有极小值.噻吩类产物中,噻吩、2-甲基噻吩、[3,2-b]并二噻吩、2-甲基[2,3-b]并二噻吩和2-甲基-3-巯基噻吩分别在水分含量为75％、55％、85％、65％和15％时达到最大值.

The essential oil from the Sabina chinensis L. leaves and its seeds were extracted by steam distillation and analyzed by GC-MS technique. 74 compounds whose relative mass fraction is greater than 0. 028% were identified,accounting for 99. 25% of the essential oil from the Sabina chinensis L. leaves. The main constituent of the essential oil is Phellandrene( 13. 713%),and the other main constituents are L-bornyl acetate( 10. 490%),L-4-terpineol( 10. 163%),Limonene( 9. 447%),Terpinene( 5. 134%), πPinene( 4. 397%),Terpilene( 3. 424%),Terpinolen( 2. 776%),Germacrene D( 2. 628%),( +)-Epi-bicyclosesquiphellandrene( 2. 342%),respectively. 61 compounds whose relative mass fraction is greater than 0. 037% were identified,accounting for 92. 667% of the essential oil from the Sabina chinensis L. seeds. The main constituent of the essential oil is Phellandrene( 20. 281%),and the other main constituents are L4terpineol( 11. 190%),Germacrene D( 10. 677%),Limonene( 8. 750%),πPinene( 6. 865%),Terpinene( 3. 481%),Thunbergene( 3. 141%),Terpinolen( 2. 914%),1RπPinene( 2. 652%),Terpilene( 2.164%),1-Isopropyl-4-methylbicyclo[3.1.0]hex-2-ene( 2.017%),respectively.

We have measured the rate of saponification of ethyl acetate (CH3COOC2H5) in 2,6-lutidine (2,6-DMP) + water (H2O) near and far away from its critical point by electrical conductivity experiment. We found that the rate of saponification slowed in the one-phase region at temperatures near the critical point. This behaviour is evidence in support of critical slowing down. Moreover, the experimental results were compared with those of the same reaction in a different critical mixture of 2-butoxyethanol + H2O [Y.W. Kim, Int. J. Thermophys. 25, 1025 (2004)].

Water-distilled essential oil from flowers of Magnolia grandiflora L.were analyzed by using gas chromatography-mass spectrometry(GC-MS) technique.80 Compounds with relative mass fraction more than 0.10% were identified,accounting for 96.42% of the essential oil.The main constituent of the essential oil is β-gurjunene,accounting for 10.17% of the essential oil,and the other main constituents are β-cubebene(8.90%),β-elemene(6.64%),eremophilene(5.47%),phenylethyl alcohol(4.20%),farnesol(3.94%),germacrone(2.96%),β-himachalene(2.85%),trans-nerolidol(2.85%),alloaromadendrene(2.59%),corymbolone(1.95%),caryophyllene(1.94%),tau.-muurolol(1.83%),isocadinene(1.81%),cadinol(1.77%),geraniol(1.59%),α-elemene(1.34%),farnesene(1.27%),n-hexadecanoic acid(1.12%),caryophyllene oxide(1.10%),juniper camphor(1.10%),longipinocarvone(1.09%),etc.The essential oil had good antioxidant effect,and the antioxidant activity enhanced with the concentration increasing.

We have measured the rate of SN1 hydrolysis reaction of 2-bromo-2-methylpropane in triethylamine+D2O near and far away from its critical point by electrical conductivity experiment. We report the observation of critical slowing down in the rate of reaction in the one-phase region near the consolute point of triethylamine+D2O, in contrast to Kim and Baird, J. Phys. Chem. A 107, 8435 (2003), who reported speeding up in the one-phase region of triethylamine+H2O. Like them, however, we observed slowing down in the rate of reaction in the two-phase region near the consolute point.

As the food material, the clerodeudrou trichotomum thunb leaves have rich nutrient components and precious herb values. The essential oil from the Clerodeudrou trichotomum Thunb leaves was extracted by steam distillation and analyzed by GC -MS technique. 20 compounds whose relative mass fraction is greater than 0.50% were identified, accounting for 99.57% of the essential oil. The main constituent of the essential oil is 1-Octen-3-ol （ 38.17% ）, the other main constituents are Linalool （11.73%）, Benzothiazole （9.41%） , 5 - Methyl - furfural （ 6. 85% ） , Terpineol （ 6. 79% ） ,3 - Hexen - 1 - ol （5.49%）, Benzene acetaldehyde （4. 01% ）, 2 - Hexenol （ 2. 93% ）, 2 - Aeetyl - 4 - methylphenol （2.65%） and 1-Hexanol （2.24%） ,respectively.

探讨了在141±2℃下,反应时间对抗坏血酸-谷胱甘肽(ASA-GSH)模式反应形成香味化合物的影响。挥发物中鉴定出43种香味化合物,结果表明含硫挥发物如噻吩类、脂环多硫化物、噻唑类、硫醇类和噻吩并噻吩类是此反应的主要成分。噻吩类、吡嗪类、硫醇类、噻吩并噻吩类和香味化合物总量随反应时间的延长挥发物的量逐渐增多,到200min时达到最大。相反,噻唑类随反应时间的延长挥发物的量一直缓慢递减。

The potassium hydroxide in the amino acid solution,followed by adding 38% formaldehyde,2mol/L of sodium hydrosulfide solution under 0℃,fully stirred and then allowed to naturally rise to room temperature overnight,were synthesized N-1,3,5-dihydrodithiazinyl acetic acid,2-(N-1,3,5-dihydrodithiazinyl)propanoic acid and 3-phenyl-2-(N-1,3,5-dihydrodithiazinyl)propanoic acid,yields were 77. 2%,73. 7% and 67. 1%. Structures of these compounds by IR,MS and 1H NMR testing techniques were characterized,and their fragrance was taken for a preliminary evaluation. The results showed that they all had sulfur-like,tropical fruit-like flavor characteristics,the threshold value of 18. 5～30. 7mg·kg-1.

The identification of aroma compounds, generated from model reaction of L-ascorbic acid and L-cysteine was performed using a solid-phase microextraction-gas chromatography-mass spectrometry technology. The effects of the small amount of Fe 2+ -ions, Zn 2+ -ions or Cu 2+ -ions on aroma compounds generation from model system of L-ascorbic acid and L-cysteine were investigated. The classification of aroma compounds was not affected much by Fe 2+ -ions, Zn 2+ -ions or Cu 2+ -ions, but the yield of each type of aroma compounds was decreased observably. The yield of each type of aroma compounds appeared to be affected much more by Cu 2+ -ions than by Zn 2+ -ions or Fe 2+ -ions depended on the different ions concentration. A plausible explanation for this phenomenon was that Fe 2+ -ions, Zn 2+ -ions or Cu 2+ -ions depressed the thermal degradation of L-cysteine, on the other hand, but stimulated the active intermediates to convert high molecular weight compounds.

The extraction and identification of volatile compounds,generated from Maillard reaction of Ascorbic Acid and Cysteine was performed using a solid-phase microextraction-gas chromatography-mass spectrometry(SPME-GC-MS) technology.The effect of different SPME bers,extraction temperature and extraction time on Extraction Quantity(GC-TIC peak areas) of volatile compounds was studied.The optimal SPME sampling condition was that reaction products were extracted for 50min in headspace model at 40℃ by using a CAR / PDMS(75μm thickness) ber.68 volatile compounds were identified,including ketones,furans,thiophenes,thiazoles,pyrazines,pyrroles,pyridines,thiols,phenols and multi-sulfides.Thiophenes,thiazoles and multi-sulfides,accounting for over 91% of the total mass of volatile compounds,were major components.

基于193 nm ArF准分子激光器与四级杆电感耦合等离子体质谱联用,我们描述了固体样品分析中定量校准的基本原理,提出了一个简单,快速、同时分析水系沉积物中主量及痕量元素的方法:无内标校准法.分析了水系沉积物中主、痕量共52种元素.对水系沉积物标准参考物质GSD-4的分析,结果与推荐值具有良好的一致性,相对误差<15%的有46个元素,<10%的有36个元素;大多数元素的相对标准偏差<10%.结果表明,运用多个外标和无内标校准法,能够对水系沉积物样品进行多元素快速、同时分析,分析结果的准确度优于传统的外标-内标结合校准法.

OBJECTIVE The Polygonum flaccidum Messin is a kind of tradition inside herb medicine of China,having good foreground of development in plant source agrochemical,medicine,food additive et al.The purpose of this study from the molecular level understanding of its chemical composition of active ingredients for a more rational development and utilization of these resources.METHODS The volatile compounds of Polygonum flaccidum Messin were isolated with steam distillation,and identified by capillary GC/MS and the relative contents of the constituents were determined by area nomalization method.RESULTS Fifty volatile components were identified and determined,accounting for 97.84% of the total area of the peaks.CONCLUSION The main volatile compounds are: N-(2-Aminoethyl)aziridine,3,4,5,6-Tetrahydrophthalic anhydride,3-Hexene-1-ol,Hydrogen chloride,2-Methyl-2-tert-butyl-1,3-dithiane,1-Methyl-7-oxoheptyl 2-formyl-4,6-dimethoxybenzoate,Thienobenzofuran,Phosphoric acid,diundecyl methyl ester,Phenanthrene,9-ethyl,Methyl hydrogen disulfide,Cyclopropene,1-bromotrifluoro,2-[4-(Dimethylamino)phenyl]-3-hydroxy-4H-chromen-4-one.

The volatile compounds of Patrinia villosa Juss were isolated with steam distillation, and identified by capillary GC/MS method. Fifty-one volatile components were identified and determined, was 95.77 % of the total area of the peaks. 2-Ethyl-5-methylfuran (50.97 %), Hexyl disulfide (9.47 %),1-Hexane thiol (6.97 %), Perillaldehyde(3.65 %), Humulane-1,6-dien-3-ol (2.65 %), (Z,E)-a-Farnesene (2.62 %), rans-Cary ophyllene (2.41 %), Linolenic acid, methyl ester (2.03 %), Perilla alcohol (1.63 %), Phthalic acid, diisobutyl ester (1.43 %), (-)-Camphor (1.21 %), a-Cedrol(1.16 %), Phthalic acid, mono-(2-ethylhexyl)ester (1.07 %), Borneol (1.06 %), 6-Aminoisoquinoline (1.03 %) accounted for most of them.

The volatile compounds of Toona sinensis Roem were isolated with steam distillation and identified by capillary GC/MS method.53 volatile components were identified and determined,accounting for 92.34% of the total peak area.The main volatile compounds and their relative contents are:α-cadinol(4.89%),α-selinene(5.67%),α-cubebene(5.49%),1,5-cyclodecadiene,1,5-dimethyl-8(1-methylethenyl)(5.37%),naphthalene,1,2,3,5,6,8a-hexahydro-4,7-dimethyl-1-isopropyl(5.88%),2,4,4-trimethyl-3-hydroxymethyl-5-(3-methyl-2-butene-1-yl)-cyclohexene(5.65%),nerolidol(4.97%),1-isopropyl-4-methyl-7-methylene-1,2,3,4,4a,5,6,7-octahydronaphthalene(5.87%),phytol(4.86%),1,3,6-heptatriene,2,5,6-trimethyl(4.31%),5,6-decadien-3-yne,5,7-diethyl(3.14%),1-pentene,3-ethyl-2-methyl-(2.86%),4-penten-2-ol(2.09%),2-butene,2-methyl-(2.83%),2-methyl-5-hexen-3-ol(2.99%),propiolactone(2.63%),3-hexen-1-ol(2.41%),1-pentanol,3,4-dimethyl(2.34%).

The optimum extracting conditions of red pigment in Zingiber mioga Rosc were studied by single factor analysis and orthogonal test L16(45). And the stability of the red pigment was analyzed. Results showed that: The optimum extracting conditions are: the ratio of material to solution is 1:20, the extracting temperature is 50 ℃, pH 1, the extracting time is 120 min; The red pigment resistant to heat, acid, oxidant, and common food additives, such as cane sugar, VC, amylum and citric acid, and in-resistant to light, reductant, and common food additives, such as sodium benzoate, potassium sorbate; Its stability to metal ion is high such as: Fe3+, Al3+, Ca2+ can add its color, Cu2+ can change its color, and Mg2+, K+ and Na+ can not badly affect it at all.

Objective To study the chemical components of volatile oil from Perilla frutescens(L.).Methods The volatile compounds of Toona Sinensis Roem were isolated with steam distillation,and identified by capillary GC/MS method.Results 87 volatile components were identified and determined,accounting for 99.38% of the total area of the peaks.The relative contents of the constituents were determined by area nomalization method.Conclusion The main volatile compounds are:Perillaldehyde(49.14%).In addition to aldehyde,alcohols,alkene,ester material,there is compound with N,P,S,X(X=F,Cl,Br,I)...etc.chemical elements in volatile oil.

The total Se content and the Se content in the volatile compounds was determined respectively by the method of atomic absorption spectrometer for Paederia scandens. The volatile compounds of Paederia scandens were isolated with steam distillation,and identified by capillary GC-MS method. 33 volatile components were identified and determined, accounting for 91.76% of the total area of the peaks. The relative contents of the constituents were determined by area nomalization method. The main volatile compounds are: β-propiolactone, dimethyl sulphone, acetoin, analgin, 2,4,6-cycloheptatrien-1-one,2,3- dimethyl, 3-buten-2-one, 4-butanediol monoacrylate, trans-1,2:4,5-diepoxy-p-menthane, N-methanesulfonylimidazole.

The voltammetric behavior of diclofenac sodium on the MWNT modified electrode was investigated by cyclic voltammetry and linear sweep voltammetry,and an electrochemical method for the direct determination of diclofenac sodium was established.In 0.1 mol/L HClO4 solution,the oxidation peak potential of diclofenac sodium is 0.38 V(vs Ag/AgCl),and the peak current is linear with its concentration in the range of 2.0×10-7～7.0×10-6 mol/L.The detection limit is about 9.0×10-8 mol/L for 3 min accumulation.The relative standard deviation(n=10) is 4.5% for 5.0×10-6 mol/L diclofenac sodium.Diclofenac sodium in voltain tablets was determined by this method.

Organoleptic compounds in Musa acuminata were extracted by general steam distillation, separated by means of GC and identified by GC-MS-DS. Twenty components have been identified. The key organoleptic compounds were 3-Hexen-1-ol, Bicyclo[2.2.1]heptan-2-one, 1,7,7-trimethyl-,(1R)-, Bicyclo[2.2.1]heptan-2-ol, 1,7,7-trimethyl-,(1s-endo)-, Eugenol, Benzene, 1,2-dimethoxy-4-(2-propenyl-).