Comparison of different extraction methods for the determination of α‐ and β‐thujone in sage (Salvia officinalis L.) herbal tea

Salvia officinalis L. (sage) is an important industrial plant used both for food and pharmaceutical purposes. The terpene fraction of this plant is responsible for many of its therapeutic and culinary properties. We used different extraction methods Tenax TA® purge and trap, headspace (HS) solid‐phase microextraction, HS sorptive extraction, and stir bar sorptive extraction to analyze the terpene fraction extracted from sage tea by GC–MS. Twenty compounds were identified, including α‐, β‐thujone, and several other oxygenated monoterpenes (1,8‐cineole, linalool, camphor, boneol, and bornyl acetate) and oxygenated sesquiterpenes (caryophyllene oxide, viridiflorol, humulene epoxide I, II, and III). Tenax TA® and HS sorptive extraction extracted a lower number of identified compounds, whereas HS solid‐phase microextraction allowed the complete extraction of volatiles with particular reference to α‐ and β‐thujone. The importance of the determination of thujones content in sage herbal tea is also discussed.     

Enantiomeric purity of (+/-) -methyl jasmonate in fresh leaf samples and commercial fragrances

The enantiomeric purity of (+/-) -methyl jasmonate in fresh leaf material of Jasminum from different species and Rosmarinus officinalis was examined by solid-phase microextraction-GC-MS (SPME-GC-MS). For comparison with these natural products, commercial jasmine and rosemary fragrances were also studied. The extraction conditions were selected as a result of testing different values of temperature (40, 50, and 60 degrees C) and time (2, 15, 30, and 40 min). The results obtained in this work revealed a range of enantiomeric excesses for (+/-) -methyl jasmonate varying from 13 to 95% depending on the Jasminum specie considered. In contrast, (-) -methyl jasmonate always occurred as a pure enantiomer in all R. officinalis samples studied. This implies those Jasminum species in which the enantiomeric purity of (-) -methyl jasmonate is high enough and any R. officinalis sample might be used as natural sources of pure (-) -methyl jasmonate. Concerning the commercial fragrances, those of jasmine showed enantiomeric composition of (-) -methyl jasmonate ranging from 1 to 15% whereas those of rosemary exhibited practically the pure (-) -methyl jasmonate. This fact suggests the addition and nonaddition of the racemic mixture of methyl jasmonate to the commercial jasmine and rosemary samples, respectively.     

Study of quantitative and qualitative variations in essential oils of Sicilian Rosmarinus officinalis L.

In this study the chemical characterisation of 10 Sicilian Rosmarinus officinalis L. biotypes essential oils is reported. The main goal of this work was to analyse the relationship between the essential oils yield and the geographical distribution of the species plants. The essential oils were analysed by GC-FID and GC-MS. Hierarchical cluster analysis and principal component analysis statistical methods were used to cluster biotypes according to the essential oils chemical composition. The essential oil yield ranged from 0.8 to 2.3 (v/w). In total 82 compounds have been identified, these represent 96.7–99.9% of the essential oil. The most represented compounds in the essential oils were 1.8-cineole, linalool, α-terpineol, verbenone, α-pinene, limonene, bornyl acetate and terpinolene. The results show that the essential oil yield of the 10 biotypes is affected by the environmental characteristics of the sampling sites while the chemical composition is linked to the genetic characteristics of different biotypes.     

WHITE ASPARAGUS HARVEST DATE DISCRIMINATION USING NIRS TECHNOLOGY

Asparagus is still an important resource for mid-size and small farms. It has been traditionally believed that factors such as the asparagus harvesting date have an influence on its quality. This research sought to identify the harvesting dates of different fruits by using Near Infrared Spectroscopy (NIRS) technology as quality indicators and the best zone a long of the asparagus to acquire the spectrum. All the asparagus tested came from the same manufacturer but had been canned on three different dates, giving a total of nine lots. There were one hundred asparagus per lot and the experiment data were taken from three different parts (tip, middle, and base) of each spear. Reflectance spectrum in the near infrared between 800–1700 nm was determined. Differences NIRS among the asparagus harvested on different dates were found. NIRS technology was able to classify the asparagus correctly in terms of harvest dates (71% well classified). The base of the asparagus turned out to be the best part to use in order to establish the harvest date.     

A new heterocyclic compound from Cyathula officinalis Kuan

<正>A new heterocyclic compound,named 5,5'-diisobutoxy-2,2'-bifuran(1),and four known compounds(2-5) were isolated from the roots of Cyathula officinalis Kuan.Their structures were elucidated by spectroscopic methods.Among these compounds,5,5'- dibutoxy-2,2'-bifuran(2) was isolated for the first time from this plant.     

Thermophysical Investigations of the Polymorphous Phases of Calcium Carbonate

1. Results of thermodynamic and kinetic investigations for the different crystalline calcium carbonate phases and their phase transition data are reported and summarized (vaterite: V; aragonite: A; calcite: C). A→C: T _tr=455±10°C, Δ_tr H=403±8 J mol^–1 at T _tr, V→C: T _tr=320–460°C, depending on the way of preparation,Δ_tr H=–3.2±0.1 kJ mol^–1 at T _tr,Δ_tr H=–3.4±0.9 kJ mol^–1 at 40°C, S _V ^Θ= 93.6±0.5 J (K mol)^–1, A→C: E _A=370±10 kJ mol^–1; XRD only, V→C: E _A=250±10 kJ mol^–1; thermally activated, iso- and non-isothermal, XRD 2. Preliminary results on the preparation and investigation of inhibitor-free non-crystalline calcium carbonate (NCC) are presented. NCC→C: T _tr=276±10°C,Δ_tr H=–15.0±3 kJ mol^–1 at T _tr, T _tr – transition temperature, Δ_tr H – transition enthalpy, S ^Θ – standard entropy, E _A – activation energy. 3. Biologically formed internal shell of Sepia officinalis seems to be composed of ca 96% aragonite and 4% non-crystalline calcium carbonate. This revised version was published online in July 2006 with corrections to the Cover Date.     

Comparison of the volatile constituents of different parts of Cortex magnolia officinalis by GC‐MS combined with chemometric resolution method

Volatile compositions of different parts (stem, branch and root barks) of Cortex magnolia officinalis, cultivated in China, were investigated for the first time by GC‐MS with the help of heuristic evolving latent projection (HELP). Identification of components was conducted by similarity matching to NIST mass library but also assisted by comparison of temperature‐programmed retention indices (PTRIs) with the data web available. A total of 90, 82 and 76 volatile compounds in the essential oils of the three samples taken from the same batch aforementioned were qualitatively and quantitatively determined, representing 84.03, 83.68 and 83.10% of the total content, respectively. Among the constituents determined, there were 50 components coexisting. Eudesmol and its isomers were shown to be the principal compounds in the studied samples, accounting for 47.66, 36.74 and 36.31%, respectively. The three kinds of isomers (α‐, β‐ and γ‐eudesmol) in houpo volatile oils have been tentatively qualified and quantified simultaneously for the first time. By comparative analysis, significant qualitative and semi‐quantitative differences and similarities were observed among the three samples. The results achieved provide a scientific evidence for further exploitation of Magnolia bark and clinical medication.     

Rapid analysis of constituents of Radix Cyathulae using hydrophilic interaction‐reverse phase LC‐MS

A hydrophilic interaction chromatography (HILIC) and reverse‐phase liquid chromatography (RPLC) coupled with electrospray TOF MS method was developed for the analysis and characterization of constituents in the radix of Cyathula officinalis Kuan. Separation parameters of HILIC such as buffer pH, mobile phase strength, and organic modifier were evaluated. Fructose, glucose, and sucrose were identified by HILIC‐ESI/TOF MS. Reverse‐phase liquid chromatography‐ESI/TOF MS were applied for quick and sensitive identification of major saponins in Cyathula officinalis. In‐source collision‐induced dissociation has been performed to elucidate the fragmentation pathways of oleanane‐, hederagenin‐, and gypsogmin‐type saponins. Twelve saponins were characterized in this plant for the first time, and four of them were presumed to be new compounds. In addition, one phytoecdysteroid (cyasterone) and one coumarin (6,7‐dimethoxycoumarin) were detected at the same time. The present method was capable of rapid characterizing and providing structure information of constituents from herbal drugs.     

Two new indole alkaloids from Nauclea officinalis

Two new indole alkaloids,4-oxo-4,12-dihydroindolo[2,3-a]quinolizine-3-carbaldehyde(1)and 1,6,7-trihydro-indolo-[2,3- a]furan[3,4-g]quinolizine-3,4(13H)-dione(2),were isolated from Nauclea officinalis.Their structures were determined on the basis of 1D and 2D NMR spectral data.     

黄土区金盏菊幼苗对Pb/Cd次生非生物胁迫响应的红外光谱研究

植物修复法是重金属污染场地修复的重要手段,这种"绿色修复技术"得到了学者们的广泛关注和期待。在重金属胁迫条件下,植物自身会出现相应的响应反映,进而逐渐适应并有效减缓重金属的直接毒害作用。这种微尺度的调控行为往往多维度和不可见,需要借助精密仪器分析技术加以剖析。现阶段,相关方面的研究还略显欠缺。以黄土修复植物金盏菊幼苗为研究对象,分析Pb/Cd复合胁迫对其表观形貌的影响,采用傅里叶变换红外光谱法(FTIR)识别其地下和地上部分样本的官能团性质,初步推断金盏菊对Pb/Cd胁迫的响应途径和耐受机制。研究表明:随着Pb/Cd胁迫程度的加剧,金盏菊根冠弯曲萎缩,根毛数量明显减少,而其地上部分形貌差异很小。Pb/Cd胁迫对金盏菊幼苗地下和地上部分的FTIR图谱影响较大:3 573cm~(-1)附近的—OH峰强减弱且发生移动,随着Pb/Cd胁迫浓度的增加,峰形更趋复杂化;这表明Pb/Cd与—OH间存在配位结合效应,Pb/Cd胁迫干扰了有机物的合成和分泌。饱和C—H振动峰整体红移,可能与细胞膜的膜脂氧化程度有关。1 631和1 574 cm~(-1)处吸收峰强下降,说明与之关联的蛋白质组分特性可能有异。1 385 cm~(-1)处峰位有所偏移,推测金盏菊通过改变果胶质和油脂的甲基化程度,完成细胞组织对Pb/Cd胁迫的"直接排斥→逐步适应→增强抗逆性"的过程转变。FTIR对于识别土壤重金属的植物修复机制具有重要指导意义。