scholarly journals An Optimized SPME-GC-MS Method for Volatile Metabolite Profiling of Different Alfalfa (Medicago sativa L.) Tissues

Molecules ◽  
2021 ◽  
Vol 26 (21) ◽  
pp. 6473
Author(s):  
Dong-Sik Yang ◽  
Zhentian Lei ◽  
Mohamed Bedair ◽  
Lloyd W. Sumner
Keyword(s):  
Solid Phase ◽  
Glandular Trichomes ◽  
Ambient Air ◽  
Extraction Time ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature ◽  
Buffer Solution ◽  
Biochemical Basis ◽  
Volatile Metabolites ◽  
Stems And Leaves

Solid-phase microextraction (SPME) was coupled to gas chromatography mass spectrometry (GC-MS) and a method optimized to quantitatively and qualitatively measure a large array of volatile metabolites in alfalfa glandular trichomes isolated from stems, trichome-free stems, and leaves as part of a non-targeted metabolomics approach. Major SPME extraction parameters optimized included SPME fiber composition, extraction temperature, and extraction time. The optimized SPME method provided the most chemically diverse coverage of alfalfa volatile and semi-volatile metabolites using a DVB/CAR/PDMS fiber, extraction temperature of 60 °C, and an extraction time of 20 min. Alfalfa SPME-GC-MS profiles were processed using automated peak deconvolution and identification (AMDIS) and quantitative data extraction software (MET-IDEA). A total of 87 trichome, 59 stem, and 99 leaf volatile metabolites were detected after background subtraction which removed contaminants present in ambient air and associated with the fibers and NaOH/EDTA buffer solution containing CaCl2. Thirty-seven volatile metabolites were detected in all samples, while 15 volatile metabolites were uniquely detected only in glandular trichomes, 9 only in stems, and 33 specifically in leaves as tissue specific volatile metabolites. Hierarchical cluster analysis (HCA) and principal component analysis (PCA) of glandular trichomes, stems, and leaves showed that the volatile metabolic profiles obtained from the optimized SPME-GC-MS method clearly differentiated the three tissues (glandular trichomes, stems, and leaves), and the biochemical basis for this differentiation is discussed. Although optimized using plant tissues, the method can be applied to other types of samples including fruits and other foods.

The Optimization and HS-SPME/GC-MS Analysis in Pear Fruit

2014 ◽  
Vol 1033-1034 ◽  
pp. 762-766 ◽  
Author(s):  
Guo Peng Li ◽  
Li Jing Lin ◽  
Jun Zhao ◽  
Ji Hua Li
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Extraction Time ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature ◽  
Pear Fruit ◽  
Volatile Analysis ◽  
Different Types

Solid-phase microextraction (SPME) is a rapid sample preparation in volatile analysis. The aromatic volatile compositions of ‘Kuerle’ were analyzed using SPME and gas chromatography-mass spectrometry (GC-MS). The effect of different types of fibers, extraction time, and extraction temperature on the volatile results were compared and discussed. The results were as followed. Results showed that 65μm PDMS/DVB fiber had the best effect of extraction. The optimum factors such as extraction time and temperature were 45 min and 40°C.

scholarly journals Gradual Optimization of Headspace Solid-Phase Microextraction Conditions of Volatiles in Pepper Chicken Soup Combined with Gas Chromatography-Mass Spectrometry and Principal Component Analysis

2019 ◽  
Vol 2019 ◽  
pp. 1-11
Author(s):  
Qiuyue Geng ◽  
Ping Zhan ◽  
Honglei Tian ◽  
Peng Wang ◽  
Haitao Chen
Keyword(s):  
Mass Spectrometry ◽  
Principal Component Analysis ◽  
Gas Chromatography ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Principal Component ◽  
Sample Volume ◽  
Extraction Time ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature

A single-factor gradual optimization method was developed in this experiment in order to improve the headspace solid-phase microextraction (HS-SPME) effect of volatile compounds in pepper chicken soup. The different extraction conditions included fibers with different coating materials, sample volume, extraction temperature, and extraction time. The total peak areas and the numbers of valid peaks were compared and analyzed as the indicators of condition optimization. Gas chromatography-mass spectrometry (GC-MS) results showed that the four factors all have significant impact on the extraction effect of volatiles in pepper chicken soup. Using the principal component analysis (PCA), the optimal conditions of HS-SPME were inferred below: an extraction fiber of 50/30μm DVB/CAR/PDMS, a sample volume of 7 g, an extraction temperature of 65°C, and an extraction time of 30 min. Compared to the original extraction conditions, the optimized conditions were especially advantageous for the comprehensive analysis of volatiles, which could be potentially used in further study of soup.

Optimization of HS-SPME for GC-MS Analysis of Volatiles Compounds in Roasted Sesame Oil

2014 ◽  
Vol 881-883 ◽  
pp. 61-64
Author(s):  
Zhao Xi Fang ◽  
Guo Qin Liu ◽  
Xue De Wang ◽  
Li Juan Han ◽  
Bing Ge Liu
Keyword(s):  
Solid Phase Microextraction ◽  
Capillary Column ◽  
Solid Phase ◽  
Sesame Oil ◽  
Operating Conditions ◽  
Extraction Time ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature ◽  
Volatiles Compounds

This paper was to develop a simple and rapid headspace solid-phase microextraction (HS-SPME) method coupled with gas chromatography–mass spectrometry (GC-MS) for the determination of volatiles compounds from the roasted sesame oil (RSO). A HP-5MS capillary column (30 m × 0.25 mm I.D. × 0.25 mm film thick) was used for GC-MS, and a 50/30 μm divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber was used to extract volatiles compounds. The condition was optimized by varying the sample-to-headspace ratio (0.5-2.5 g/15 ml), extraction time (10-50 min) and Splitless time (0.5-4 min). The results showed that the optimal operating conditions occurred at (extraction temperature:40°C, sample-to-headspace ratio: 1.5 g/15 ml, extraction time: 40 min, Splitless time: 1 min) for the analyze method.

Development of a Headspace-Solid Phase Micro Extraction Method for the Analysis of Volatile and Semi-Volatile Organic Compounds from Polyurethane Resins for Leather Finishing

2021 ◽  
Vol 116 (8) ◽  
Author(s):  
Antonia Flores ◽  
Silvia Sorolla ◽  
Concepció Casas ◽  
Rosa Cuadros ◽  
Anna Bacardit
Keyword(s):  
Gas Chromatography ◽  
Volatile Organic Compounds ◽  
Organic Compounds ◽  
Solid Phase ◽  
Monomethyl Ether ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature ◽  
Solid Phase Micro Extraction ◽  
Volatile Organic ◽  
Leather Finishing

Volatile organic compounds (VOCs) and Semi-Volatile Organic Compounds (SVOCs) arise from the chemicals used in the various stages of the leather manufacturing process. An important aim of the tanning industry is to minimize or eliminate VOCs and SVOCs, without lowering the quality of leather.   This paper shows the development of a new headspace-solid phase micro extraction coupled with gas chromatography–mass spectrometry (HS-SPME/GC-MS) method for the identification of VOCs and SVOCs emitted by newly designed polymers for the leather finishing operation. These new polymers are polyurethane resins designed to reduce the VOC and SVOC concentration. This method enables a simple and fast determination of the qualitative and semi-quantitative content of VOCs and SVOCs in polyurethane-type finishing resins. The chemicals that are of concern in this paper are the following: Dipropylene glycol Monomethyl Ether (DPGME), DBE-3 (a mixture of dibasic esters) and Triethylamine (TEA). The test conditions that have been determined to carry out the HS-SPME assay are the following: incubation time (2 hours), extraction temperature and time (40°C; 5 minutes) and the desorption conditions (280°C, 50 seconds).  Ten samples of laboratory scale resins were tested by HS-SPME followed by gas chromatography (GC-MS). DPGME and DBE-3 (a mixture of dimethyl adipate, dimethyl glutarate and dimethyl succinate) have been identified effectively. The compounds are identified by a quantitative method using external calibration curves for the target compounds. The technique is not effective to determine the TEA compound, since the chromatograms shown poor resolution peaks for the standard. 

scholarly journals Quantitative and enantioselective analysis of monoterpenes from plant chambers and in ambient air using SPME

2010 ◽  
Vol 3 (6) ◽  
pp. 1615-1627 ◽  
Author(s):  
N. Yassaa ◽  
T. Custer ◽  
W. Song ◽  
F. Pech ◽  
J. Kesselmeier ◽  
...  
Keyword(s):  
Competitive Adsorption ◽  
Solid Phase ◽  
Ambient Air ◽  
Enantiomeric Separation ◽  
Gas Chromatography Mass Spectrometry ◽  
Peak Resolution ◽  
Whole Plant ◽  
Fibre Coating ◽  
Chamber Studies ◽  
Spme Fibre

Abstract. A headspace solid-phase microextraction (HS-SPME) and gas chromatography/mass spectrometry (GC/MS) system has been developed for quantifying enantiomeric and nonenantiomeric monoterpenes in plant chamber studies and ambient air. Performance of this system was checked using a capillary diffusion system to produce monoterpene standards. The adsorption efficiency, competitive adsorption and chromatographic peak resolution of monoterpene enantiomer pairs were compared for three SPME fibre coatings: 75 μm Carboxen-PDMS (CAR-PDMS), 50/30 μm divinylbenzene-carboxen-polydimethylsiloxane (DVB-CAR-PDMS) and 65 μm divinylbenzene-polydimethylsiloxane (DVB-PDMS). Key parameters such as the linearity and reproducibility of the SPME system have been investigated in this work. The best compromise between the enantiomeric separation of monoterpenes and competitive adsorption of the isoprenoids on the solid SPME fibre coating was found for DVB-PDMS fibres. The optimum conditions using DVB-PDMS fibres were applied to measure the exchange rates of monoterpenes in the emission of Quercus ilex using a laboratory whole plant enclosure under light and dark conditions, as well as in ambient air. With 592 and 223 ng m−2 s−1 respectively, β-myrcene and limonene were the predominant monoterpenes in the emission of Q. ilex. These values were closely comparable to those obtained using a zNose and cartridge GC-FID systems.

scholarly journals Volatile Compounds from Roots, Stems and Leaves of Angelica acutiloba growing in Taiwan

2014 ◽  
Vol 9 (4) ◽  
pp. 1934578X1400900 ◽  
Author(s):  
Hsin-Chun Chen ◽  
Yi-Jr Tsai ◽  
Li-Yun Lin ◽  
Chin-Sheng Wu ◽  
Shan-Pao Tai ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Volatile Compounds ◽  
Solid Phase Microextraction ◽  
Oil Content ◽  
Steam Distillation ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Stems And Leaves ◽  
Angelica Acutiloba

The present study analyzed and compared the volatile compounds in fresh Angelica acutiloba roots, stems and leaves both qualitatively and quantitatively. The volatile compounds were isolated by either steam distillation (SD) or headspace-solid phase microextraction (HS-SPME). A total of 61 compounds were identified using gas chromatography/mass spectrometry (GC/MS). All 61 compounds were verified by SD, with 3n-butyl phthalide, γ-terpinene, p-cymene and cis-β-ocimene as the main compounds. Thirty-three compounds were verified by HS-SPME, with γ-terpinene and p-cymene as the main compounds. The leaf samples contained the highest essential oil content. Compared with SD, HS-SPME sampling resulted in relatively higher amounts of highly volatile monoterpenes and lower amounts of less volatile compounds such as 3n-butyl phthalide. These findings demonstrate that A acutiloba roots, stems and leaves have high 3 n-butyl phthalide contents; thus, all parts of A. acutiloba may be used for further application and development.

Optimization of Solid Phase Microextraction (SPME) Coupled with Gas Chromatography Mass Spectrometry (GC-MS) for Fermented Perilla Leaves Jiaosu and Volatile Profiling Analysis During Fermentation

2020 ◽  
Vol 14 (3) ◽  
pp. 359-368
Author(s):  
Ruyi Sha ◽  
Haoan Fan ◽  
Zhenzhen Wang ◽  
Gaojian Wang ◽  
Yanli Cui ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Volatile Compounds ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Volatile Components ◽  
Extraction Temperature ◽  
Spontaneous Fermentation ◽  
Chromatography Mass Spectrometry

A method based on solid phase microextraction coupled with gas chromatography mass spectrometry was developed for volatile profiling fermented perilla leaves jiaosu (PFJ) during fermentation. Five fibers were firstly evaluated by the total peak areas and the number of volatile compounds. Secondly, a Plackett-Burman design was applied to screen for seven independent variables selected in literature. Three significant variables (extraction time, extraction temperature and equilibrium time) were therefore selected for the following optimization studies. A Box-Behnken design combined with a steepest ascent was then used to optimize the significant factors. Under optimal conditions, the changes of volatile profiles of PFJ at 7, 14, 21, 28, 91 and 140 d were analyzed. A total of fifty-one volatile compounds were identified, and alcohols (68.12–78.94%) were the main volatile components in PFJ, followed by methoxy-phenolic compounds (4.67–5.48%). Perilla alcohol and trans-Shisool were the major constituents during spontaneous fermentation, which accounted for 16.14–30.66% and 19.95–24.52%, respectively. The results showed that PFJ fermented into a health probiotic product with characteristic flavour and functional volatile compounds.

Analysis of 16 phthalate esters in wastewater from textile plants using headspace solid-phase microextraction and gas chromatography with mass spectrometric detection

2020 ◽  
pp. 004051752094190
Author(s):  
Ying Li ◽  
XiWen Ye ◽  
ZengYuan Niu ◽  
Jing He ◽  
Xin Luo ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Salt Concentration ◽  
Solid Phase Microextraction ◽  
Matrix Effects ◽  
Solid Phase ◽  
Phthalate Esters ◽  
Extraction Time ◽  
Extraction Temperature ◽  
Textile Processing ◽  
Processing Plants

Solid-phase microextraction (SPME) with a 100-µm polydimethylsiloxane (PDMS) fiber coupled to gas chromatography–mass spectrometry was used to determine 16 phthalate esters (PAEs) in wastewater from textile processing plants. Some of the 16 PAEs that exist as mixtures of isomers were identified and quantified. We investigated the matrix effect and evaluated a qualification and quantitation method for determining trace amounts of PAEs in wastewater from textile processing plants. The major advantages of this approach are the reduced matrix effects from the textile wastewater and the compatibility with the standard addition method (SAM) for PAE quantitation. Moreover, the developed method has low reagent and solvent consumption, does not require clean-up or evaporation steps and involves minimal sample manipulation. Two fiber coatings, 85-µm polyacrylate and 100-µm PDMS, were tested. The variables affecting SPME absorption, such as the sample temperature, extraction time and salt concentration, were studied. The final conditions were an extraction temperature of 95℃, an extraction time of 30 min and a salt concentration of 0.3 g/mL. The SAM was used to analyze and quantify samples. The linear range was between 5 and 20 µg/L, and the limits of detection of the method were between 0.5 and 5 µg/L. Finally, the precision of the phthalate quantitation was also evaluated.

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