Analysis of Rhioxma Curcumae Aeruginosae Volatiles by Solid-phase Microextraction with Gas Chromatography-Mass Spectrometry

2004 ◽  
Vol 59 (7-8) ◽  
pp. 533-537 ◽  
Author(s):  
Yun F. Sha ◽  
Shun Shen ◽  
Geng L. Duan
Keyword(s):  
Volatile Compounds ◽  
Solid Phase Microextraction ◽  
Steam Distillation ◽  
Solid Phase ◽  
Good Alternative ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature ◽  
Good Reproducibility ◽  
Volatile Constituents ◽  
Relative Standard

AbstractIn this paper, a headspace solid-phase microextraction (HS-SPME) method was applied to analyse the volatile compounds in a traditional Chinese medicine (TCM), Rhioxma Curcumae Aeruginosae. SPME parameters such as fibers, extraction temperature, extraction time and desorption time were investigated. Thirty-five volatile compounds were separated and identified. Relative standard deviations (RSDs) were less than 8.4%, showing that the method has a good reproducibility. The volatile constituents were also analyzed by steam distillation (SD) and thirty-seven compounds were identified. The similar results obtained by the two methods showed that SPME is a good alternative for the analysis of volatile constituents in Rhioxma Curcumae Aeruginosae samples and it is a relatively simple, rapid and solvent-free method.

scholarly journals Comparison of Solid-Phase Microextraction, Supercritical Fluid Extraction, Steam Distillation, and Solvent Extraction Techniques for Analysis of Volatile Consituents in Fructus Amomi

2005 ◽  
Vol 88 (2) ◽  
pp. 418-423 ◽  
Author(s):  
Shun Shen ◽  
Yunfei Sha ◽  
Chunhui Deng ◽  
Daxi Fu ◽  
Jiakuan Chen ◽  
...  
Keyword(s):  
Solvent Extraction ◽  
Supercritical Fluid Extraction ◽  
Supercritical Fluid ◽  
Solid Phase Microextraction ◽  
Steam Distillation ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature ◽  
Fluid Extraction ◽  
Volatile Constituents

Abstract Four sampling techniques, solid-phase microextraction (SPME), supercritical fluid extraction (SFE), steam distillation (SD), and solvent extraction (SE), were compared for the analysis of volatile constituents from a traditional Chinese medicine (TCM) of the dried ripe fruit of Fructus Amomi (Sha Ren). A total of 38 compounds were identified by gas chromatography/mass spectrometry. Different SFE and SPME parameters (modifier content, extraction pressure, and temperature for SFE and fibers, extraction temperature, and time for SPME) were studied. The results by SFE and SPME were compared with those obtained by conventional SD and SE methods. The results showed that SFE and SPME are better sample preparation techniques than SD and SE. Due to SFE's requirement for expensive specialized instrumentation, the simplicity, low cost, and speed of SPME make it a more appropriate technique for extraction of volatile constituents in TCMs.

scholarly journals Identification of Volatile Compounds in Chrysanthemum morifolium by Microwave Distillation Solid-Phase Microextraction Coupled with GC/MS

2009 ◽  
Vol 92 (3) ◽  
pp. 855-861 ◽  
Author(s):  
Tao Zhou ◽  
Bei Yang ◽  
Haiying Zhang ◽  
Yingjia Yu ◽  
Bin Chen ◽  
...  
Keyword(s):  
Volatile Compounds ◽  
Solid Phase Microextraction ◽  
Steam Distillation ◽  
Solid Phase ◽  
Irradiation Time ◽  
Chrysanthemum Morifolium ◽  
Single Step ◽  
Water Volume ◽  
Relative Standard ◽  
Microwave Distillation

Abstract Microwave distillation with concomitant solid-phase microextraction (MD-SPME) coupled with GC/MS was developed for identifying volatile compounds in the dried flowers of Chrysanthemum morifolium (CM). Different experimental parameters, including SPME fiber coating, microwave power, irradiation time, and water volume were optimized. The best results were obtained using carboxen/polydimethylsiloxane fiber with microwave irradiation at 400 W for 3 min and the addition of 1 mL water into 1.0 g sample. The proposed method allowed the isolation, extraction, and concentration of volatile compounds to be completed in a single step. This MD-SPME-GC/MS method has also been compared to the conventional steam distillation method followed by GC/MS for this identification. Thirty-two volatile compounds were identified using the newly developed MD-SPME-GC/MS process. Relative standard deviation values of <9.8 demonstrate good repeatability. In comparison, 27 compounds were identified by traditional steam distillation-GC/MS. Therefore, the proposed MD-SPME-GC/MS method is simple, rapid, and efficient for identifying volatile compounds in CM.

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.

scholarly journals Analysis of Volatile Compounds in Probiotic Yogurt during Storage through Solid-phase Microextraction Gas Chromatography

2019 ◽  
pp. 1-11
Author(s):  
Ana Cristina Tanello ◽  
Cristine Durante de Souza Silveira ◽  
Eduardo Carasek ◽  
Silvani Verruck ◽  
Elane Schwinden Prudencio ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Volatile Compounds ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Influential Factors ◽  
Hexanoic Acid ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature ◽  
Refrigerated Storage ◽  
Probiotic Yogurt

Two different yogurts, control and probiotic with Bifidobacterium BB-12 were produced and analyzed for their contents of total solids, proteins, pH, counts of probiotic bacteria, and volatile composition during refrigerated storage for 28 days. The response surface methodology (RSM) was used to optimize the extraction of volatile compounds from the probiotic yogurt containing through HS-SPME combined with gas chromatography–mass spectrometry (GC–MS). Post-acidification and decrease in protein content were noted in both yogurts during storage. The results showed that the extraction temperature and the addition of salt were statistically the most influential factors for the extraction of higher amounts of volatile compounds. The volatile compounds detected in the probiotic yogurt were 2-butanone, 2,3-butanedione, 2,3-pentanodione, acetone and hexanoic acid. During the 28 days of storage, the only differences noted were between the amounts of 2,3-butanedione, 2,3-pentanodione and hexanoic acid.

scholarly journals Processing of Flavor-Enhanced Oils: Optimization and Validation of Multiple Headspace Solid-Phase Microextraction-Arrow to Quantify Pyrazines in the Oils

Life ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 390
Author(s):  
Ziyan Xu ◽  
Chuan Zhou ◽  
Haiming Shi ◽  
Hong Zhang ◽  
Yanlan Bi ◽  
...  
Keyword(s):  
Solid Phase Microextraction ◽  
Incubation Temperature ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature ◽  
Headspace Solid Phase Microextraction ◽  
Flavor Analysis ◽  
Relative Standard ◽  
Limit Of Quantitation

An efficient and effective multiple headspace-solid phase microextraction-arrow-gas chromatography-mass spectrometry (MHS-SPME-arrow-GCMS) analytical protocol is established and used to quantify the flavor compounds in oils. SPME conditions, such as fiber coating, pre-incubation temperature, extraction temperature, and time were studied. The feasibility was compared between SPME-arrow and the traditional fiber by loading different sample amounts. It was found that the SPME-arrow was more suitable for the MHS-SPME. The limit of detection (LODs) and limit of quantitation (LOQs) of pyrazines were in the range of 2–60 ng and 6–180 ng/g oil, respectively. The relative standard deviation (RSD) of both intra- and inter-day were lower than 16%. The mean recoveries for spiked pyrazines in rapeseed oil were in the range of 91.6–109.2%. Furthermore, this newly established method of MHS-SPME-arrow was compared with stable isotopes dilution analysis (SIDA) by using [2H6]-2-methyl-pyrazine. The results are comparable and indicate this method can be used for edible oil flavor analysis.

scholarly journals A multi internal standard calibration approach for the automated and robust analysis of wine volatiles by headspace Solid Phase Microextraction and further Gas Chromatography-Mass Spectrometry

1970 ◽  
pp. 34
Author(s):  
P. Herrero ◽  
J. Zapata ◽  
J. Cacho ◽  
Vicente Ferreira
Keyword(s):  
Volatile Compounds ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Relative Weight ◽  
Experimental Parameter ◽  
Internal Standard ◽  
Partial Least Square ◽  
Least Square ◽  
Gas Chromatography Mass Spectrometry ◽  
Volatile Constituents

Head space solid phase microextraction (HS-SPME) is a solvent-free technique that allows an almost complete automatization and getting amazing sensitivities. The hidden risk of SPME lies in the fact that as the amount of analyte extracted is very low; it is extremely sensitive to any experimental parameter that may affect the liquid-gas and gas-solid distribution coefficients. Our aims are to measure the relative weight of these factors on the lack of accuracy, and to design a robust calibration system able to avoid or limit their effects.For the first goal, synthetic but real-like wines containing a fixed amount of selected analytes (70) and variable amounts of ethanol, non-volatile constituents and major volatile constituents were prepared following a 3-Factor complete Factorial design. The study of the relevance of the Factors carried out by analysis of variance (ANOVA) and by Principal Component Analysis revealed that the levels of major volatile constituents affected the extraction of most analytes, while ethanol and matrix affected particularly low volatile compounds. Lipophilic esters are most influenced by major volatile compounds, while acids, phenols and lactones are affected by the non-volatile matrix.13 different internal standard compounds belonging to different chemical classes were used in the calibration experiment. This was similar to the aforementioned experiment, but including as well 5 different concentration levels. In 29 out of 65 cases, a single internal standard provided a robust calibration guaranteeing an accuracy better than 10%, while in others a Partial Least Square Regression analysis was run in order to find a model able to provide maxima accuracy. Satisfactory models in terms of precision, linearity and recovery could be built for 30 other compounds, so that the method can quantify up to 59 relevant wine volatile compounds.

scholarly journals Solid-Phase Microextraction Arrow for the Sampling of Volatile Organic Compounds in Milk Samples

Separations ◽  
2020 ◽  
Vol 7 (4) ◽  
pp. 75
Author(s):  
Natalia Manousi ◽  
Erwin Rosenberg ◽  
George A. Zachariadis
Keyword(s):  
Volatile Organic Compounds ◽  
Organic Compounds ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature ◽  
Milk Samples ◽  
Relative Standard ◽  
Wide Range ◽  
Volatile Organic

A novel sample preparation method based on the use of the Arrow solid-phase microextraction device was used to extract and preconcentrate volatile organic compounds (VOCs) from milk samples prior to their determination by gas chromatography–mass spectrometry (GC-MS). The experimental parameters of the solid-phase microextraction (SPME) Arrow method were evaluated in terms of fiber type, sample volume, extraction temperature, extraction time, stirring rate and salt addition. Under the optimum extraction conditions, the SPME Arrow was compared with conventional SPME fibers to evaluate the effectiveness of the SPME Arrow method. Evaluation of the conventional SPME procedure was also performed under optimized conditions, for appropriate method comparison. Due to the larger sorption phase volume of SPME Arrow, a higher sensitivity and reproducibility were observed for the determined chromatographic peaks in comparison with conventional SPME fibers. The use of Carbon wide range (WR) SPME Arrow/polydimethylsiloxane (CAR/PDMS) SPME Arrow fibers leads to a compound-dependent improvement of a factor of 4–5x over the classical SPME setup. Moreover, the relative standard deviation (RSD) of the total volatiles for a conventional SPME procedure was 12.5%, while for SPME Arrow it was 6.2%. Finally, the novel method was successfully employed for the analysis of commercially available milk samples. The findings of this study indicate that SPME Arrow can be effectively used for the determination of volatile organic compounds in complex food matrixes.

scholarly journals Characterization of Volatile Compounds in Tom Yum Soup by Headspace-Solid Phase Microextraction-Gas Chromatography-Mass Spectrometry Combined with Sensory Evaluation Techniques

2018 ◽  
Author(s):  
Pannipa Janta ◽  
Chadin Kulsing ◽  
Thumnoon Nhujak
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Volatile Compounds ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Temperature ◽  
Headspace Solid Phase Microextraction ◽  
Before And After

Gas chromatography-olfactometry/mass spectrometry coupled with headspace-solid phase microextraction (HS-SPME/GC-O/MS) was applied for the characterization of volatile compounds in Tom Yum soup and its individual ingredients. Using HS-SPME with a 50/30 µm DVB/CAR/PDMS fiber and an extraction temperature of 40 °C for 50 min along with an HP-5MS capillary column, 101 peaks in the HS-SPME/GC-MS chromatogram of Tom Yum soup were detected, and 96 compounds were identified including alcohols, aldehydes, esters, ethers, and terpenes. These findings are based on the comparison of MS spectra with the NIST library as well as experimental and literature retention index data. In comparison with the compound profiles of each individual ingredient of Tom Yum soup (both before and after cooking), five extra volatile compounds in Tom Yum soup were found after the cooking process. Furthermore, odor descriptions of the eighteen aroma compounds in Tom Yum soup, along with the odor ingredient sources, were also obtained.

scholarly journals Determination of multi-class herbicides in soil by liquid-solid extraction coupled with headspace solid phase microextraction method

2016 ◽  
Vol 81 (8) ◽  
pp. 923-934 ◽  
Author(s):  
Rada Djurovic-Pejcev ◽  
Tijana Djordjevic ◽  
Vojislava Bursic
Keyword(s):  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Soil Samples ◽  
Gas Chromatography Mass Spectrometry ◽  
Optimum Number ◽  
Polydimethyl Siloxane ◽  
Headspace Solid Phase Microextraction ◽  
Relative Standard ◽  
Detection And Quantification

A method is described for simultaneous determination of five herbicides (metribuzin, acetochlor, clomazone, oxyfluorfen and dimethenamid) belonging to different pesticides groups in soil samples. Developed headspace solid phase microextraction method (HS-SPME) in combination with liquid-solid sample preparation (LS) was optimized and applied in the analysis of some agricultural samples. Optimization of microextraction conditions, such as temperature, extraction time and sodium chloride (NaCl) content was perfor-med using 100 ?m polydimethyl-siloxane (PDMS) fiber. The extraction effi-ciencies of methanol, methanol:acetone=1:1 and methanol:acetone:hexane= =2:2:1 and the optimum number of extraction steps during the sample prepa-ration, were tested, as well. Gas chromatography-mass spectrometry (GC-MS) was used for detection and quantification, obtaining relative standard deviation (RSD) below 13%, and recovery values higher than 83% for multiple analyses of soil samples fortified at 30 ?g kg-1 of each herbicide. Limits of detection (LOD) were less than 1.2 ?g kg-1 for all the studied herbicides.

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