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.

scholarly journals Determination of Low-Level Residual Ethylene Oxide by Using Solid-Phase Microextraction and Gas Chromatography

2002 ◽  
Vol 85 (6) ◽  
pp. 1205-1209 ◽  
Author(s):  
Kamal Ayoub ◽  
Leonard Harris ◽  
Bill Thompson
Keyword(s):  
Gas Chromatography ◽  
Ethylene Oxide ◽  
Medical Devices ◽  
Solid Phase Microextraction ◽  
Capillary Column ◽  
Solid Phase ◽  
Extraction Temperature ◽  
Absorption Time ◽  
Low Level

Abstract Current methods of analysis for ethylene oxide (EO) in medical devices include headspace and simulated-use extractions followed by gas chromatography with either a packed or a capillary column. The quantitation limits are about 0.5–1.0 μg/g for a packed column and about 0.1–0.2 μg/g for a capillary column. The current allowable levels of EO on medical devices sterilized with EO gas as outlined in International Organization for Standardization (ISO) 10993-7 may be significantly reduced from current levels by applying the ISO Draft International Standard 10993-17 method for establishing allowable limits. This may require EO test methods with detection and quantitation limits that are much lower than those of the currently available methods. This paper describes a new method that was developed for the determination of low-level EO by solid-phase microextraction using the direct-immersion method. Factors such as temperature and stirring were found to affect absorption efficiency and absorption time. A low extraction temperature (about 6°C) was found to be more efficient than room-temperature extraction. Stirring was found to reduce absorption time by about 50%. Under these conditions, detection and quantitation limits of 0.002 and 0.009 μg/g, respectively, were obtained by using a capillary column. As a result, this method makes compliance with lower EO limits feasible.

Determination of Nonylphenol and Octylphenol in Seawater Samples Using Solid-Phase Microextraction Procedures Coupled to Gas Chromatography–Mass Spectrometry

2012 ◽  
Vol 518-523 ◽  
pp. 1496-1500 ◽  
Author(s):  
Xian Yin Ping ◽  
Hui Sheng Zhuang
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Detection Limits ◽  
Operating Conditions ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Seawater Samples

The solid-phase microextraction (SPME) technique with on-fiber derivatization coupled to gas chromatography–mass spectrometry was evaluated for the analysis of technical nonylphenol (NP) and octylphenol (OP). The optimization of operating conditions influencing the performances of SPME and derivatization were studied in detail. The optimised method was linear over the range studied and showed good level of precision, with a RSD lower than 10% and detection limits at and 0.003 μgL−1for OP and 0.032μgL−1for NP, respectively. The results obtained from different seawater samples revealed the presence of the target compounds, at levels ranging between 0.034 and 0.186 μgL−1.

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.

scholarly journals Determination of atrazine, acetochlor, clomazone, pendimethalin and oxyfluorfen in soil by a solid phase microextraction method

2008 ◽  
Vol 23 (4) ◽  
pp. 265-271 ◽  
Author(s):  
Rada Djurovic ◽  
Jelena Gajic-Umiljendic ◽  
Tijana Djordjevic
Keyword(s):  
Sample Preparation ◽  
Solid Phase Microextraction ◽  
Solid Phase ◽  
Soil Samples ◽  
Extraction Time ◽  
Gas Chromatography Mass Spectrometry ◽  
Optimum Number ◽  
Extraction Solvent ◽  
Relative Standard

A solid phase microextraction (SPME) method for simultaneous determination of atrazine, acetochlor, clomazone, pendimethalin and oxyfluorfen in soil samples was developed. The method is based on a combination of conventional liquid-solid procedure and a following SPME determination of the selected pesticides. Initially, various microextraction conditions, such as the fibre type, desorption temperature and time, extraction time and NaCl content, were investigated and optimized. Then, extraction efficiencies of several solvents (water, hexane, acetonitrile, acetone and methanol) and the optimum number of extraction steps within the sample preparation step were optimized. According to the results obtained in these two sets of experiments, two successive extractions with methanol as the extraction solvent were the optimal sample preparation procedure, while the following conditions were found to be most efficient for SPME measurements: 100 ?m PDMS fibre, desorption for 7 min at 2700C, 30 min extraction time and 5% NaCl content (w/v). Detection and quantification were done by gas chromatography-mass spectrometry (GC/MS). Relative standard deviation (RSD) values for multiple analysis of soil samples fortified at 30 ?g/kg of each pesticide were below 19%. Limits of detection (LOD) for all the compounds studied were less than 2 ?g/kg.

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