In‐tube solid‐phase microextraction capillary column packed with mesoporous TiO 2 nanoparticles for phosphopeptide analysis

2019 ◽  
Vol 40 (16-17) ◽  
pp. 2142-2148 ◽  
Author(s):  
Ke Li ◽  
Shuo Zhao ◽  
Yong Yan ◽  
Dongtang Zhang ◽  
Manhua Peng ◽  
...  
2009 ◽  
Vol 4 (2) ◽  
pp. 50-59
Author(s):  
Rodica Sturza ◽  
Constantin Sîrghi ◽  
Mariana Vrîncean ◽  
Susanne Böhme

The study has been focused on the comparative analysis of various analytical techniques for the injection of samples applied to detect the additives with flavouring potential that are used to obtain illicitly the "Muscat" and "Isabela" wines, by implementing the GC/MS method with injection of liquid samples directly into the capillary column, using the "Head-space" method and the solid phase microextraction (SPME).


2002 ◽  
Vol 85 (6) ◽  
pp. 1205-1209 ◽  
Author(s):  
Kamal Ayoub ◽  
Leonard Harris ◽  
Bill Thompson

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.


2014 ◽  
Vol 881-883 ◽  
pp. 61-64
Author(s):  
Zhao Xi Fang ◽  
Guo Qin Liu ◽  
Xue De Wang ◽  
Li Juan Han ◽  
Bing Ge Liu

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.


Author(s):  
Ariza Budi Tunjung Sari ◽  
Teguh Wahyudi ◽  
Amrita Sulihkanti

The approach to authenticate Luwak coffee is made through analysis of volatile compounds of luwak coffee. Luwak coffee bean from type of arabica obtained from Andungsari Plantation in Bondowoso district, East Java Province Indonesia, was wet processed and sundried prior to roasting step. As many as 120 g green bean was roasted at 170-220°C for 8-12 minutes until reached light brown colour (Agtron scale 65) and was ground prior to extraction. Volatile compounds of roasted Luwak arabica coffee bean were extracted by using solid phase microextraction (SPME) at 60°C for 30 minutes. The extracted analyte was subsequently transferred into GC-FID system by splitless injection at 260°C with five minutes sampling time, continued with separation through 50% phenyl 50% dimethylpolysiloxane capillary column and oven temperature programmed from 60°C to 180°C with rate of 5°C/min. Resulted chromatogram shows major peaks mainly in Rt 8.360-9.981, and Rt 9.705-14.778, and minor peaks identified before Rt 10 and after Rt 24. Varied sample quantity ranged within 0.5-2.5 g produced chromatograms which were not significantly different (p=0.08). This research also observed the use of γ-picoline (4-methylpyridine) as internal standard. It was showed that γ-picoline appeared at Rt 8.6~ without overlaying other peaks originated from sample. Concentration of γ-picoline at 0.05 μL/g, resulted separable peaks. These findings showed that the use of solid phase microextraction and GC-FID is capable to be apply for identification and quantification of Luwak coffee


2016 ◽  
Vol 99 (2) ◽  
pp. 520-526 ◽  
Author(s):  
Xin Du ◽  
YongLin Ren ◽  
Stephen J Beckett

Abstract The rapid detection of pesticide residues in wheat has become a top food security priority. A solvent-free headspace solid-phase microextraction (HS-SPME) has been evaluated for rapid screening of organophosphorus pesticide (OPP) residues in wheat with high sensitivity. Individual wheat samples (1.7 g), spiked with 10 OPPs, were placed in a 4 mL sealed amber glass vial and heated at 60°C for 45 min. During this time, the OPP residues were extracted with a 50 μm/30 μm divinylbenzene (DVB)/carboxen (CAR)/plasma desorption mass spectroscopy polydimethylsiloxane (PDMS) fiber from the headspace above the sample. The fiber was then removed and injected into the GC injection port at 250°C for desorption of the extracted chemicals. The multiple residues were identified by a GC mass spectrometer detector (GC-MSD) and quantified with a GC flame photometric detector (GC-FPD). Seven spiked levels of 10 OPPs on wheat were analyzed. The GC responses for a 50 μm/30 μm DVB/CAR/PDMS fiber increased with increasing spiking levels, yielding significant (R2 > 0.98) linear regressions. The lowest LODs of the multiple pesticide standards were evaluated under the conditions of the validation study in a range of levels from 0 (control) to 100 ng of pesticide residue per g of wheat that separated on a low-polar GC capillary column (Agilent DB-35UI). The results of the HS-SPME method were compared with the QuEChERS AOAC 2007.01 method and they showed several advantages over the latter. These included improved sensitivity, selectivity, and simplicity.


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