Optimization of the Extraction Technology of Volatile Oil from Schizonepeta tenuifolia and Forsythia suspensa / 中国药房

OBJECTIVE： To establish the method for content determination of volatile oil of Schizonepeta tenuifolia and Forsythia suspensa， and to optimize the extraction technology of the volatile oil. METHODS： The contents of β-pinene and pulegone were determined by GC method. The determination was performed on Hp-5 capillary column. The detector was hydrogen flame ion detector with programmed temperature. The sample size was 0.5 μL， the split ratio was 70 ∶ 1， the carrier gas was nitrogen， the inlet temperature was 250 ℃， the detector temperature was 280 ℃， the air flow rate was 390 mL/min， the hydrogen flow rate was 36 mL/min， the tail flow rate was 15 mL/min， and the nitrogen flow rate was 1 mL/min. Based on single factor test， orthogonal test combined with information entropy method were used to optimize the extraction technology of S. tenuifolia and F. suspensa using soaking time， extraction time， material-liquid ratio and forsythia grain size as factors， with the extraction amount of volatile oil， the content of β-pinene and pulegone and their comprehensive score as indexes.  RESULTS： The linear range of β-pinene and pulegone 1.575-7.875（r＝0.999 9） and 1.892-9.46 μg（r＝0.999 7）， respectively. The limits of quantitation were 0.10 and 0.25 μg； the limits of detection were 0.03 and 0.08 μg； RSDs of precision， stability and reproducibility tests were less than 2％ （n＝6）； the recoveries were 97.77％-100.01％ （RSD＝0.93％，n＝9） and 96.47％-99.00％（RSD＝0.89％， n＝9）. The optimal extraction technology was soaking 2 h， extracting for 6 h， 10-fold water （mL/g）， half a clove of granularity. Under this condition， the extraction amount of volatile oil， the contents of β-pinene and pulegone were 3.6 mL， 1 450.4 mg， 127.6 mg， respectively. RSD were 1.62％， 0.20％， 1.42％. CONCLUSIONS： Established method is simple， accurate and reproducible， and the optimal extraction technology is stable and feasible.

Simultaneous Determination of Contents of 6 Components in the Oil of Blumea balsamifera by GC / 中国药房

OBJECTIVE： To establish a method for simultaneous determination of contents of β-pinene， linalool， L-camphor， L-borneol， β-caryophyllene and xanthoxylin in the oil of Blumea balsamifera. METHODS： GC method was adopted. The determination was performed on RTX-1701 capillary column （programmed temperature）. The FID detector was controlled at 240 ℃. The inlet temperature was set at 240 ℃. The carrier gas was high-purity nitrogen 3 mL/min. The the sample size was 0.5 μL， and split ratio was 50 ∶ 1. RESULTS： The linear range of β-pinene， linalool， L-camphor， L-borneol， β-caryophyllene and xanthoxylin were 0.029 7-0.267 1 mg/mL （r＝0.999 9）， 0.024 3-0.218 9 mg/mL （r＝0.999 9）， 0.126 0-1.134 0 mg/mL （r＝0.999 9）， 0.217 2-1.954 8 mg/mL （r＝0.999 9）， 0.136 3-1.226 9 mg/mL （r＝0.999 9）， 0.044 5-0.400 3 mg/mL（r＝0.999 5）， respectively. The limits of quantitation were 0.028 5， 0.008 7， 0.018 6， 0.016 8， 0.014 5， 0.042 1 mg/mL； the limits of detection were 0.009 4， 0.002 9， 0.006 1， 0.005 5， 0.004 8， 0.013 9 mg/mL， respectively. RSDs of precision， stability， reproducibility and durability tests were all lower than 3％. The average recoveries were 98.13％-101.30％（RSD＝1.20％，n＝9），98.44％-101.81％（RSD＝1.28％，n＝9），98.26％-101.05％（RSD＝1.19％，n＝9），99.08％-101.58％（RSD＝0.89％，n＝9），98.66％-101.66％（RSD＝1.17％，n＝9），98.84％-103.60％（RSD＝0.96％，n＝9）， respectively. The contents of 6 components in the sample were 14.552-46.766， 16.951-22.096， 80.597-113.115， 205.224-242.537， 47.761-135.697， 26.493-45.771 mg/g， respectively. CONCLUSIONS： The established method is simple， accurate， precise and reproducible， which can be used for simultaneous determination of contents of 6 components in the oil of B. balsamifera. It can provide reference for comprehensive evaluation and extraction technology study of the oil of B. balsamifera.

Feasibility of vapor permeation technology for separating of Asari Radix et Rhizoma essential oil-bearing water / 中草药

Objective: To verify the feasibility of vapor-permeable membrane technology for the separation of water bodies containing essential oil of Asari Radix et Rhizoma (ARR) essential oil, and then to apply vapor permeate technology to the separation of more essential oils of traditional Chinese medicine. Methods: The polydimethylsiloxane/polyvinylidene fluoride (PDMS/PVDF) composite flat membrane and polyvinylidene fluoride (PVDF) flat membrane were collected as the membrane material. The oil-bearing water body of ARR volatile oil was separated by vapor permeate technology, and the oil penetration rate of two kinds of membranes was calculated. At the same time, the changes of the composition and content of the essential oil before and after the membrane were analyzed by gas chromatography-mass spectrometry (GC-MS). Results: The results showed that the essential oil penetration rate was significantly higher than that of PDMS/PVDF membrane when PVDF membrane was used as membrane material. GC-MS qualitative analysis results showed that the composition of the essential oil in the penetrants of the two membranes was basically the same as that of the essential oil obtained by the traditional steam distillation method. The content of α-pinene, β-pinene, 3,5-dimethoxytoluene, and methyl eugenol were determined by double internal standard method. The results showed that the content of each component in the PVDF membrane permeation was significantly higher than that of the PDMS/PVDF membrane permeation solution. Conclusion: It is feasible to separate the oil containing water from the essential oil of ARR by vapor permeation membrane technology. Compared with the PDMS/PVDF membrane, the PVDF membrane is more suitable for separating the oil containing water of the essential oil of ARR.

Phytochemical and Antimicrobial Evaluation of the Essential Oil of Croatian Salvia brachyodon Vandas

Backgraund: This study was designed to evaluate the phytochemical profile and the antimicrobial potential of the essential oil of Salvia brachyodon Vandas growing wild in Croatia. Short tooth sage (S. brachyodon Vandas),an endemic species that grows in the south east areas of the Adriatic coast in Croatia, Bosnia and Herzegovina, and Montenegro. It is a perennial plant that grows up to 70-80 cm in height and flowers from July to September. Methodology: The phytochemical components of the essential oil were identified by gas chromatography-mass spectrometry (GC-MS) analysis. The antimicrobial activity was assessed against a panel of representative Gram-positive and Gram-negative bacteria as well as fungi. The antimicrobial activities of the oil against pathogenic microorganisms were determined by using agar disc diffusion and broth microdilution methods. Results: From the thirty-eight identified constituents representing 95.7% of the oil, 1,8-cineole (16.7%), β-pinene (19.7%) and α-pinene (7.6%), were the major components. The levels of oxygenated monoterpenes such as camphor (5.6%), borneol (4.2%), myrtenol (2.4 %) and terpinen-4-ol were significant. Other important compounds were sesquiterpenes hydrocarbons β-caryophyllene (6.6%), α-humulene (4.9%), viridiflorol (3.0%), spathulenol (2.9%) and aromadendrene. Preliminary antimicrobial screening revealed that the oil exhibited a very interesting antimicrobial profile. The oil exhibited moderate in vitro antibacterial activity after it was tested against twenty pathogenic bacteria and fungal strains, but high antimicrobial activity observed against medically important pathogens such as E. coli O157:H7, Listeria monocytogenes and Candida albicans. Conclusion: Results presented here may suggest that the essential oil of S. brachyodon possess antimicrobial properties, and is, therefore, a potential source of antimicrobial ingredient in food and pharmaceutical industry. The obtained results are preliminary and a further research is needed in order to obtain information regarding the practical effectiveness of essential oil to prevent the growth of foodborne and spoilage microbes under specific application conditions.

Simultaneous Determination of α-pinene,β-pinene and Linalool in Volatile Oil from Hedychium flavum by GC / 中国药房

OBJECTIVE:To establish a method for simultaneous determination of α-pinene,β-pinene and linalool in volatile oil of Hedychium flavum. METHODS:The volatile oil was extracted from H. flavum according to steam distillation stated in Chinese Pharmacopoeia(2015 edition volume Ⅳ). GC method was adopted to determine the content. The determination was performed on HP-5 capillary chromatographic column(30 m×0.032 mm×0.25 μm)with hydrogen flame ion detector(FID),nitrogen gas as carrier gas,with injector temperature of 200 ℃,and detector temperature of 250 ℃,column flow rate of 0.8 mL/min, samples size of 1 μL and split ratio of 40:1 by programmed temperature. RESULTS:The linear range of α-pinene,β-pinene and linalool were 0.090 5-2.413 3 mg/mL(r=0.999 9),0.098 3-2.620 0 mg/mL(r=0.999 9),0.169 1-4.510 0 mg/mL(r=0.999 8), respectively. RSDs of precision,stability(12 h),reproducibility tests were no more than 2.0%(n=6). The average recoveries were 99.84%(RSD=0.49%,n=6),100.24%(RSD=1.38%,n=6),99.41%(RSD=1.67%,n=6),respectively.The contents of α-pinene,β-pinene and linalool ranged 0.214 4-1.325 0,0.766 2-3.172 1,0.357 4-1.518 7 mg/g in volatile oil from 23 batches of H. flavum produced in Guizhou province. CONCLUSIONS:The method established in this experiment is rapid,simple and accurate.It can be used for the content determination of α-pinene,β-pinene and linalool in volatile oil from H.flavum.

Comparative Analysis on Simultaneous Determination of α-pinene, β-pinene, Eucalyptol and Linalool in Baeckea Frutescens Preparations by Reference Substances Method and Reference Extract Method / 中国中医药信息杂志

Objective To determinate the contents of α-pinene, β-pinene, eucalyptol and linalool in Baeckea frutescens by reference substances method and reference extract method respectively; To explore the feasibility of replacing single component reference by control extracts in assay. Methods The GC system consisted of a quartz column DB-5 (60 m×0.25 mm×0.25 μm); The temperature programming rose from 80 ℃ (15 min) to 90 ℃ by 1 ℃/min, lasting 2 min, then 10 ℃/min to 110 ℃, then 25 ℃/min to 240 ℃, lasting 8 min in the end; The temperature of the entrance of capillary vessel column was 250 ℃, and the temperature of the detector was 250 ℃. Results α-pinene, β-pinene, eucalyptol and linalool were in a good linear relationship within each concentration scope (r≥0.999). The average recovery rates were in the range of 96.5%–102.2%. The results of t-test demonstrated that there is no significant difference between the two methods. Conclusion The reference extract method can be used as a quality evaluation pattern for Baeckea frutescens.

Chemical Composition of the Leaf Essential Oils of Croton zambesicus Müll.-Arg. Grown in Lagos, South-West Nigeria.

The chemical composition of the leaf essential oil of Croton zambesicus Müll.-Arg., collected from Agbara-Lagos, Nigeria, was analysed by means of Gas chromatography flame ionization detector (GC-FID) and Gas chromatography coupled with Mass spectrometry (GC-MS). Sixty constituents accounting for 98.9% of the total oil contents were identified from the oil sample. The classes of compounds identified in the oil were monoterpene hydrocarbons (35.3%), oxygenated monoterpenes (22.9%), sesquiterpene hydrocarbons (32.4%) and oxygenated sesquiterpenes (5.6%). The oil was dominated by β-pinene (15.1%), β-caryophyllene (12.6%), germacrene D (10.9%), camphor (7.3%), linalool (7.0%), sabinene (6.4%) and α-pinene (5.2%). Aims: The aim of the research is to investigate the volatile constituents from C. zambesicus harvested in Lagos, Nigeria. Study Design: Extraction of essential oil from the air-dried leaf samples of C. zambesicus and investigation of its chemical constituents. Place and Duration of Study: Leaf samples of C. zambesicus were collected from Agbara, Lagos, on April 2011. Methodology: Air-dried and pulverized leaves were hydrodistilled in a Clevenger-type apparatus to obtained pale yellow volatile oil whose chemical constituents was analyzed by GC and GC/MS. Results: A total of sixty compounds were identified, amounting to 98.9%of the total oil contents. The major were compounds β-pinene (15.1%), β-caryophyllene (12.6%), germacrene D (10.9%) and camphor (7.3%). Variations in compositional pattern were observed between this result and the previous studies. Conclusion: The literature about the C. zambesicus indicates a high variability in the chemical composition of the essential oils.

Analysis of the Essential Oil of the Germander (Teucrium Polium L.) Aerial Parts from the Northern Region of Saudi Arabia.

The chemical composition of the essential oil of the aerial parts of Teucrium polium L. collected during the flowering period from, northern region of Saudi Arabia, (Aljuf, kingdom of Saudi Arabia) has been studied by GC and GC/MS. 114 compounds were identified amounted to 88.51% of the total oils. The presence of sesquiterpenoid hydrocarbons (34.62%) characterizes the oil of Saudi Arabian germander. While, T. polium oil is also rich with hydrocarbons monoterpenes (26.08%), oxygenated monoterpenes (11.14%) and oxygenated sesquiterpenoids (11.79%). The dominant constituents (52.17%) wereγ-muurolene (8.72%), α-cadinol (5.93%), δ-cadinene (5.08%), β -pinene (4.58 %), β-gurjurene (4.43 %), α-limonene (4.29 %), α-Pinene (3.79 %),α-Thujene (3.69%), Spathulenol (3.42 %), p-cymene (2.95%) γ-cadinene (2.81%)and Sabinene (2.47 %).