To identify the 6-PP molecule using a standard method, we performed a Solid-Phase Microextraction (SPME) on days 3 and 5. The fiber (fused silica fiber plain blue hub for volatiles) was exposed for 1 h. The injection sample port was at 230 °C to introduce the compounds in an Agilent 19091S-433 HP-5 ms column. GC-MS detected VOCs in the following conditions: start at 45 °C with a gradient of 9 °C/min up to 250 °C, maintaining the temperature for 1 min, and decreasing it to 220 °C, as described in [11 (link)]. The data were compared to the National Institute of Standards and Technology (NIST) 2008 database, with Enhanced ChemStation (v. F.01.01.2317) from Agilent Technologies with a spectra similarity of 87.4% [31 ].
19091s 433 hp 5 ms column
Manufactured by Agilent Technologies
The 19091S-433 HP-5 ms column is a gas chromatography (GC) column designed for the separation and analysis of a wide range of organic compounds. It features a 30-meter length, 0.25-millimeter internal diameter, and a 0.25-micrometer film thickness. The column is made of fused silica and coated with a 5% phenyl-methylpolysiloxane stationary phase, which provides excellent separation capabilities for a variety of analytes.
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4 protocols using 19091s 433 hp 5 ms column
1
Identification of 6-PP Molecule using SPME-GC-MS
2
Bioactive Profile Analysis by GC-MS
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For a quantitative analysis of bioactive profiles from all crude extracts, Hewlett-Packard (HP) 6890 GC MS was used with Agilent 19091S-433 HP-5MS column having 30 m length and 250 µm id. Helium was used as carrier gas at flow rate of 1 mL/min and oven temperature was set at 325°C. The initial oven temperature was 150°C which was held at 1°C/min. It ran for 10°C/min and was later increased to 240°C hold time for 2 min. The total run time was 22 minutes. The scan range was 50 - 550 amu. Structural assignments were based on analysis of fragmentation pattern of mass spectra and direct comparison of mass spectra with profiles in the National Institute of Standards and Technology (NIST) and Wiley library.
3
GC-MS Analysis of JCEO Compounds
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Gas Chromatography–Mass Spectrometry (GC-MS) was conducted to identify the compounds in the extracted JCEO. This analysis used an Agilent 6890N Network Gas Chromatograph equipped with an Agilent 19091S-433HP-5MS column, with dimensions of 30 m × 0.25 mm × 0.25 µm. First, 1 µL of the essential oil was injected into the GC inlet, and then a column flow rate of 1.3 mL/min was maintained. Initially, the column temperature was established at 325 °C, and the injection temperature was set to 280 °C. The oven temperature was programmed to increase from 65 °C to 450 °C at a rate of 3 °C per min. Subsequently, the detector scanning was conducted for a duration of 45 min. The identification of the reported individual components was achieved through a comparison of the mass spectra and by referring to the GC-MS library.
4
GC-MS Analysis of Citrus reticulata Peel Extract
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Following conditions were adopted for gas chromatography-mass spectrometry (GC-MS) analysis.[20 ] The component identification was done using Agilent 7890 A gas chromatograph coupled with 5975 C inert Mass Selective Detector (MSD) with Triple Axis Detector. Samples were injected by Agilent 7693 auto sampler into Agilent 19091S-433: HP-5MS column (30 m × 250 μm × 0.25 μm). Helium was used as a carrier gas (1 ml/min). Injector and detector temperature were kept at 250°C. Column temperature was programed at 60°C for 3 min and then raised up to 160°C for 2 min at 10°C/min. Further temperature was raised up to 300°C (at 15°C/min). Mass spectra were acquired over 40–500 amu range in EI mode. The eluted compounds were identified by comparing mass spectral data with the standard data available in the library of National Institute of Standards and Technology. Main constituents from Soxhlet methanolic extract of C. reticulata Blanco peel (CR HAE) were identified by GC-MS analysis.
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