scholarly journals Gıdalarda Uçucu Bileşen Analizinde Katı Faz Mikroekstraksiyon Koşullarının Optimizasyonunda Yanıt Yüzey Yönteminin Kullanılması

Author(s):  
Ceyda Dadalı ◽  
Yeşim Elmacı Elmacı

High vacuum steam distillation, simultaneous distillation extraction, steam distillation, purge and trap methods are used for sample preparation in volatile component analysis. Since these methods are difficult and costly to implement, these methods have left their place to the solid phase microextraction technique. Extraction conditions such as extraction temperature, extraction time, sample volume and fiber type should be optimized in order to increase the efficiency of extraction in volatile component analysis with solid phase microextraction in foods. In the optimization of extraction conditions in volatile component analysis of foods, studies have been carried out to utilize the response surface method, which reduces the number of experiments and also examines the interaction effect of the independent variables. In this review, it is aimed to give information about current studies using response surface methodology in optimization of volatile compound analysis of foods using solid phase microextraction technique.

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.


2012 ◽  
Vol 95 (1) ◽  
pp. 222-226 ◽  
Author(s):  
Maurizio Boccacci Mariani ◽  
Vanessa Giannetti ◽  
Elena Testani ◽  
Virginia D'Aiuto

Abstract The formation of organohalogen compounds in waters treated by chlorination has drawn increasing scientific attention due to the potentially hazardous health effects of this class of substances. Today, chlorination is the most widely used technology for civil water disinfection. In this study, headspace- solid phase microextraction coupled with GC-electron capture detector was used to determine organohalogen compounds in drinking water sampled from aqueducts and artesian wells in Italy. Experimental parameters, such as sample volume, stirring, salting out, extraction temperature, and extraction time, were evaluated and optimized. The LODs ranged from 1 to 10 ng/L and LOQs from 5 to 50 ng/L. A linear response was confirmed by correlation coefficients ranging from 0.9443 to 0.9999. Quantifiable organohalogen residues were found in 11 water samples, with concentration up to 11.3 ± 0.5 μg/L for the sum of all trihalomethanes and 0.66 ± 0.03 μg/L for the sum of trichloroethylene and tetrachloroethylene. These concentrations are lower than the current regulatory limits in Italy.


2019 ◽  
Vol 2019 ◽  
pp. 1-11
Author(s):  
Qiuyue Geng ◽  
Ping Zhan ◽  
Honglei Tian ◽  
Peng Wang ◽  
Haitao Chen

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.


2017 ◽  
Vol 100 (1) ◽  
pp. 218-223 ◽  
Author(s):  
Nasim Mohammadnezhad ◽  
Amir Abbas Matin ◽  
Naser Samadi ◽  
Ashkan Shomali ◽  
Hassan Valizadeh

Abstract Linear ionic liquid bonded to fused silica and its application as a solid-phase microextraction fiber for the extraction of bisphenol A (BPA) from water samples were studied. Afteroptimization of microextraction conditions (15 mL sample volume, extraction time of 40 min, extraction temperature of 30± 1°C, 300 μL acetonitrile as the desorption solvent, and desorption time of 7 min), the fiber was used to extract BPA from packed mineral water, followed by HPLC–UV on an XDB-C18 column (150 × 4.6 mm id, 3.5 μm particle) with a mobile phase of acetonitrile–water (45 + 55%, v/v) and flow rate of 1 mL . min−1). A low LOD (0.20 μg. L−1) and good linearity (0.9977) in the calibration graph indicated that the proposed method was suitable for the determination of BPA.


2005 ◽  
Vol 88 (2) ◽  
pp. 418-423 ◽  
Author(s):  
Shun Shen ◽  
Yunfei Sha ◽  
Chunhui Deng ◽  
Daxi Fu ◽  
Jiakuan Chen ◽  
...  

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.


2013 ◽  
Vol 2013 ◽  
pp. 1-8 ◽  
Author(s):  
Zhisheng Xie ◽  
Qundi Liu ◽  
Zhikun Liang ◽  
Mingqian Zhao ◽  
Xiaoxue Yu ◽  
...  

Volatile components fromExocarpium Citri Grandis(ECG) were, respectively, extracted by three methods, that is, steam distillation (SD), headspace solid-phase microextraction (HS-SPME), and solvent extraction (SE). A total of 81 compounds were identified by gas chromatography-mass spectrometry including 77 (SD), 56 (HS-SPME), and 48 (SE) compounds, respectively. Despite of the extraction method, terpenes (39.98~57.81%) were the main volatile components of ECG, mainly germacrene-D, limonene, 2,6,8,10,14-hexadecapentaene, 2,6,11,15-tetramethyl-, (E,E,E)-, andtrans-caryophyllene. Comparison was made among the three methods in terms of extraction profile and property. SD relatively gave an entire profile of volatile in ECG by long-time extraction; SE enabled the analysis of low volatility and high molecular weight compounds but lost some volatiles components; HS-SPME generated satisfactory extraction efficiency and gave similar results to those of SD at analytical level when consuming less sample amount, shorter extraction time, and simpler procedure. Although SD and SE were treated as traditionally preparative extractive techniques for volatiles in both small batches and large scale, HS-SPME coupled with GC/MS could be useful and appropriative for the rapid extraction and qualitative analysis of volatile components from medicinal plants at analytical level.


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.


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