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Gas Chromatography - Mass Spectrometry (GC-MS) analysis of
Volatile oils
By:
Nourhan Hani
Under supervision:
Dr.Nouran Mohamed
Introduction
Methods & Material
Conclusion
Result & Discussion
Nourhan.hani9019@pharma.asu.edu.eg
Introduction
Overview
Overview
Gas chromatography mass spectrometry (GC/MS) is an instrumental technique, comprising a gas chromatograph (GC) coupled to a mass spectrometer (MS), by which complex mixtures of chemicals may be separated, identified and quantified. This makes it ideal for the analysis of the hundreds of relatively low molecular weight compounds found in environmental materials.
In order for a compound to be analysed by GC/MS it must be sufficiently volatile and thermally stable.
Early development of the technique owes a good deal to the pioneering efforts of Gohlke and McClafferty during the1950s at The Dow Chemical Company (Dow).
The Process
The Process
Gas Chromatography Mass Spectroscopy is when a small sample of the analysis substance is introduced into a gas stream (the carrier gas) flowing through a column packed with solid material coated in a liquid. Then the time taken for the substance to pass through the column is recorded, this is the retention time.
The detector records the retention time and quantity of the substances as they leave the column. The mass spectrometer identifies and quantifies the chemicals.
Advantages
GC/MS has advantages over LC/MS in
1- Peak capacity.
2- Chromatographic resolution.
3- Ruggedness/reliability.
4- The exceptional separation power of GC, often providing over 100,000 theoretical plates.
5- Readily combined with universal ionization sources such as electron ionization (EI).
Methods & Material
1.Plant Material
Plant Material
Citrus reticulata, Rutaceae, leaves and green branches were collected from Benha City, Qualyobia, Egypt in December 2012
2.Isolation of Volatile Aroma Compounds
Isolation of Volatile Aroma Compounds
The fresh leaves and branches C. reticulata were hydrodistilled in all glass Clevenger apparatus for 5 h as described by Sharma and Tripathi, 2006.
The hydrodistillation of leaves resulted in two layers, one was heavier than water and the other is lighter. Branches yielded only one lighter layer of oil. The volatile oils were dried over anhydrous sodium sulphate and stored at 5°C in the dark.
Analysis of Volatile Aroma Components by GC and GC-MS
3. GC–MS analysis was performed on a Perkin-Elmer quadrupole MS system
GC analysis was carried out using a Perkin-Elmer Autosystem apparatus equipped with FID and fused silica capillary columns (30 m X 0.25 mm i.d., film thickness 0.25 μm), HP-5 (diphenyl dimethyl polysiloxane).
Oven temperature was programmed from 45°C to 240°C at 3°C/min; injector temperature, 280°C; detector temperature, 250°C; carrier gas, helium (1ml/min); automatic sample injection, 0.02 μl of the oil; split: 1/60. The relative proportions of the essential oil constituents were expressed as percentages obtained by peak area normalization without using correcting factors.
* GC–MS analysis was performed on a Perkin-Elmer quadrupole MS system
(Model 910) coupled with the above gas chromatograph, equipped with a HP-5 capillary column and operating under the same conditions described above, except for the carrier gas flow rate (1 ml/min.). The MS operating parameters were: ionization 70 eV; ion source temperature, 230°C; sc an mass range, 35–450 Da.
4. Compounds Identification
Compounds were identified using their MS data compared to those from the NIST mass spectral library and published mass spectra (Adams, 2007).
Compounds Identification
Result & Discussion
Qualitative and quantitative analysis of the essential oils volatile profile are listed in Table 1.
These results showed that there are many qualitative similarities between the three oils although the amounts of some corresponding compounds are different.
The green branches produced dark yellow oil in a high yield 0.4 % (v/w).
Eighteen compounds were identified, which represented about 91.346 % of the total detected constituents.
The major constituents of the oil were dimethyl anthranilate (34.7 %), Y- terpinene (33.6 %) and limonene (11.2 %). Alpha pinene and sabinene were present in considerable amount (both are 2.8%). Other components were present in amounts less than 2%.
In the oil of leaves (heavier layer; pale yellow, 0.2 % v/w) thirteen compounds, accountings for 92.5 % of the oil were identified. Dimethyl anthranilate (65.3%) was the major component, followed by Y-terpinene (19.8%) and limonene (4.5 %).
The lighter layer (pale yellow, 0.3 % v/w) of mandarin leaves oil; fourteen compounds were identified (94.7%) Dimethyl anthranilate (60.6%) was also the major component, followed by Y-terpinene (22.8%) and limonene (5.3 %).
FURTHER INVESTIGATION WAS DONE ON THE SAME POINT…
“In silico and in vitro investigation of the biological activity of dimethyl anthranilate (DMA) isolated from petit grain mandarin agro-waste”
1-Extraction: Hydrodistillation of petit grain mandarin oil from agro-waste leaves yield about 5% of oil v/w . and the isolated DMA was about 99.76%.
2- Gas chromatography-Mass spectroscopy (GC-MS) : For the GC/MS analysis of petit grain mandarin oil the major components were are DMA(44.99) , C-Terpinene ,dl Limonene , Thujene , α-Pinene , Sabinene , 2α-Pinene , α-Terpinene , α-Terpinolene
Conclusion
Conclusion
- Hydrodistillation of petit grain mandarin leaves agro-waste yielded 5% volatile oil v/w which was analyzed by GC/MS.
- The major components of mandarin oil are DMA(44,99) , C-Terpinene ,dl Limonene , Thujene , α-Pinene , Sabinene , 2α-Pinene , α-Terpinene , α-Terpinolene.