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 ◽  
...  

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.

2004 ◽  
Vol 59 (7-8) ◽  
pp. 533-537 ◽  
Author(s):  
Yun F. Sha ◽  
Shun Shen ◽  
Geng L. Duan

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.


2014 ◽  
Vol 9 (4) ◽  
pp. 1934578X1400900 ◽  
Author(s):  
Hsin-Chun Chen ◽  
Yi-Jr Tsai ◽  
Li-Yun Lin ◽  
Chin-Sheng Wu ◽  
Shan-Pao Tai ◽  
...  

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.


2014 ◽  
Vol 988 ◽  
pp. 397-406 ◽  
Author(s):  
Chang Bin Wei ◽  
Xiao Dong Ding ◽  
Yu Ge Liu ◽  
Wei Feng Zhao ◽  
Guang Ming Sun

An analytical method of solid-phase microextraction (SPME) was developed for pineapple aroma volatile compounds. Different sample preparation procedures involving SPME fibres, including the addition of sodium chloride, extraction time, and temperature, were evaluated to optimise the method. For the optimised method, 6.5 g of ground pineapple flesh was placed in a 20 mL headspace vial with 1 g of sodium chloride; a 65 μm polydimethylsiloxane/divinylbenzene fibre was used for extraction at 50°C for 40 min with continuous stirring. The method was validated by determining its repeatability and recovery. The relative standard deviations for the pineapple aroma compounds were 5.48-11.02%. The average method recovery was 99.13%. The results demonstrate that this SPME procedure is suitable as a simple, rapid, and solvent-free extraction technique for the analysis of pineapple aroma volatile compounds. Using this method, 15 volatile compounds were identified, and the amount was 1019.78 μg.kg−1 in pineapple cv. Shenwan, including seven esters, one terpene, two aldehydes, one ketone, two lactones, one alcohol, and one hydrocarbon. A tentative study to estimate the contribution of the identified compounds to the aroma of the pineapple variety based of their odour activity values indicated four compounds that were characteristic aroma compounds, including methyl hexanoate, δ-octalactone, decanal, and geranyl acetone.


2018 ◽  
Vol 24 (3) ◽  
pp. 235-239 ◽  
Author(s):  
Roghayeh Hendi ◽  
Marzieh Piriyaei ◽  
Marzieh Babashpour Asl ◽  
Mir Mahdi Abolghasemi

Background: In the current study, simultaneous extraction and concentration of the analytes from the headspace on the solid phase microextraction (SPME) fiber were followed by transferring the essential oil components of Salvia hydrangea DC to the headspace with the help of a heating source. Methods: The essential oil components of the plant were extracted and concentrated in a single step. A one-at-the-time optimization procedure was applied to the microextraction conditions by using the nanocomposite fiber of polypyrrole/SBA-15. Results: The results of the essential oil extraction of Salvia hydrangea clearly demonstrated that polypyrrole/SBA-15 fibers were efficient with SPME technique. The acceptable SPME precision in our study was corroborated by the relative standard deviation (RSD) values of less than 15%. Conclusion: In comparison to the hydro-distillation (HD) method, the SPME technique could equally provide monitoring of almost all the constituents of the studied essential oil in an easier way and shorter time with much lower amounts of the plant sample. The results of the essential oil extraction of Salvia hydrangea clearly demonstrated that polypyrrole/SBA-15 fibers were efficient with SPME technique.


2007 ◽  
Vol 79 (7) ◽  
pp. 2869-2876 ◽  
Author(s):  
Charlotte N. Legind ◽  
Ulrich Karlson ◽  
Joel G. Burken ◽  
Fredrik Reichenberg ◽  
Philipp Mayer

2016 ◽  
Vol 81 (8) ◽  
pp. 923-934 ◽  
Author(s):  
Rada Djurovic-Pejcev ◽  
Tijana Djordjevic ◽  
Vojislava Bursic

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.


Author(s):  
Huiju Wang

Ionic     liquid (IL), 1-dodecyl-3-methylimidazolium-3-hydroxy-2-naphthoate (C12mimHNC) was synthesized and coated on the surface of NiTi as solid phase microextractiom fiber coating for determination the octadecylamine in brine. Prior to modification with IL, the NiTi was hydrothermally treated for in-situ growth of titanium and nickel oxide composite nanosheets (TiO2/NiOCNSs). The TiO2/NiOCNSs fibers coating was oriented  around the NiTi  substrate and  presented  double-faced  open  access  sites,  which provided a desired support framework for the further modification with IL. The extraction performance of C12mimHNC-TiO2/NiOCNSs fiber coating was evaluated for       detection of octadecylamine (ODA) coupled to HPLC with UV detection. As a result, the C12mimHNC-TiO2/NiOCNSs fiber coating illustrated excellent adsorption and extraction capability for ODA. The main factors affected extraction efficiency were optimized. Under the optimized  conditions,  good  linearity was  obtained  in  the  range of  1-150  µg/L with correlation  coefficients  (r2)  above  0.985.  Limits of detection (LODs) for  the  developed method was 0.280 µg/L. The proposed method was first applied to extract the ODA in brine samples. Relative recoveries varied from 78.3% to 96.5% at spiking level of 15µg/L and 30 µg/L with the relative standard deviations (RSDs) less than 8.7%.


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