The use of a simple backflush technology to improve sample throughput and system robustness in routine gas chromatography tandem mass spectrometry analysis of doping control samples

Gray, Bobby; Teale, P.

doi:10.1016/j.chroma.2010.05.004

Cited by 17 publications

(7 citation statements)

References 10 publications

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“…The use of the PLOT column makes backflushing essential when injecting liquid crude samples. During the backflush, the columns are heated and gas flow is reversed out the inlet, removing hydrocarbons from the column and preventing their transfer to the PLOT column during subsequent injections [25][26][27] . The process of backflushing will result in a buildup of material in the inlet liner of the GC, and the liner will require cleaning and/or replacement approximately every 50 injections.…”

Section: Discussionmentioning

confidence: 99%

“…A sulfur chemiluminescence detector is used for detection, providing selectivity for sulfur compounds and eliminating possible interference from any other light gases that may have been transferred to the PLOT column during the heart cut. Hydrocarbons from the crude oil sample are retained on the first dimension column and are removed during a backflush procedure; this protects the PLOT column from any contamination [25][26][27] . This approach has also been successfully implemented for the analysis of oxidation inhibitors in transformer oils 28 .…”

Section: Introductionmentioning

confidence: 99%

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Measurement of H<sub>2</sub>S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

Heshka

Hager

2015

JoVE

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A method for the analysis of dissolved hydrogen sulfide in crude oil samples is demonstrated using gas chromatography. In order to effectively eliminate interferences, a two dimensional column configuration is used, with a Deans switch employed to transfer hydrogen sulfide from the first to the second column (heart-cutting). Liquid crude samples are first separated on a dimethylpolysiloxane column, and light gases are heart-cut and further separated on a bonded porous layer open tubular (PLOT) column that is able to separate hydrogen sulfide from other light sulfur species. Hydrogen sulfide is then detected with a sulfur chemiluminescence detector, adding an additional layer of selectivity. Following separation and detection of hydrogen sulfide, the system is backflushed to remove the high-boiling hydrocarbons present in the crude samples and to preserve chromatographic integrity. Dissolved hydrogen sulfide has been quantified in liquid samples from 1.1 to 500 ppm, demonstrating wide applicability to a range of samples. The method has also been successfully applied for the analysis of gas samples from crude oil headspace and process gas bags, with measurement from 0.7 to 9,700 ppm hydrogen sulfide.

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Section: Discussionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Measurement of H<sub>2</sub>S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

Heshka

Hager

2015

JoVE

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“…Besides its application in the multidimensional GC , the back‐flush technique was also used in the 1D GC. The latter was carried out in different ways: back‐flushing (i) the precolumn , (ii) a part of the analytical column , or (iii) the complete analytical column . Precolumn back‐flushing is characterized by the removal of high boiling matrix compounds before entering the analytical column.…”

Section: Introductionmentioning

confidence: 99%

Application of the precolumn back‐flush technology in pesticide residue analysis: A practical view

Hildmann

Kempe²,

Speer

2013

J of Separation Science

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Precolumn back-flushing is a matrix minimization technique in GC in which the carrier gas flow of the precolumn is reversed after the transfer of the highest boiling analyte to the analytical column. Practical details concerning this technology have rarely been published although it is widely used. This paper now focuses on the practical implementation of precolumn back-flushing for pesticide residue analysis of complex food matrices. Fitting the analytical column into the precolumn was found to be essential for comparable analyte responses with and without back-flushing. The effectiveness of the reverse column flow technique is mainly affected by the transfer time after which back-flushing starts. The transfer time was found to depend on which kind of injected matrix is used and the state of the precolumn. For the regular adaptation of the transfer time in routine analysis, a simple test was introduced in which 13-C-labeled deltamethrin and indeno[1,2,3-c,d]pyrene were added to the prepared extract. Chromatograms, LOQ and RSD of up to 99 pesticides in citrus oil and liver extracts proved a clearer identification and enhanced quantification using precolumn back-flushing compared to measurements without this technology. Furthermore, reduced system maintenance could be achieved through back-flushing.

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“…In general, low content and complicated matrix are the two obstacles of the determination of pesticide residues in MFDPHs. Furthermore, the contamination of injection inlet and column by high boiling matrix compounds during GC analysis should be also considered, which could affect the chromatographic separation and reduce column life . So far, a series of sample preparation methods, including liquid–liquid extraction (LLE) , pressurized liquid extraction (PLE) , solid phase extraction (SPE) , gel permeation chromatography (GPC) , QuEChERS (quick, easy, cheap, effective, rugged, and safe) , and solid phase micro extraction (SPME) have been employed for the extraction and enrichment of pesticides in Chinese herbal medicine.…”

Section: Introductionmentioning

confidence: 99%

“…Typically, the multiple reaction monitoring of GC‐MS/MS gives the possibility of simultaneous confirmation and quantification with excellent selectivity and sensitivity. In addition, a column backflush offered potential advantages to reduce run time and prevent high boiling contaminants to GC‐MS system .…”

Section: Introductionmentioning

confidence: 99%

Rapid determination of pesticide residues in herbs using selective pressurized liquid extraction and fast gas chromatography coupled with mass spectrometry

Xiao

Yang³

et al. 2012

J of Separation Science

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A selective pressurized liquid extraction and gas chromatography coupled with triple quadrupole mass spectrometer method was developed for simultaneous determination of 52 pesticide residues in medicine and food dual-purpose herbs. The developed extraction method integrated extraction and cleanup processes for sample preparation. The sorbents, 5 g Florisil and 100 mg graphitized carbon black, were placed inside the extraction cell to remove matrix interferences. Optimized conditions of selective pressurized liquid extraction were ethyl acetate as extraction solvent, 120°C of extraction temperature, 6 min of static extraction time, 50% of flush volume extracted for two cycles. An ultra inert capillary GC-MS HP-5 UI column (20 m × 0.18 mm id, 0.18 μm) and column backflush system were used for the analysis. Multiple-reaction monitoring was employed for the quantitative analysis with electron ionization mode. All calibration curves showed good linearity (r(2) > 0.995) within the test ranges. The average recoveries of most pesticides were from 81 to 118%. The validated method was successfully applied for the determination of pesticide residues in four herbs. The results indicate that selective pressurized liquid extraction and GC-MS/MS is a sensitive and reliable analytical method for the simultaneous determination of multiple pesticide residues in herbs.

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The use of a simple backflush technology to improve sample throughput and system robustness in routine gas chromatography tandem mass spectrometry analysis of doping control samples

Cited by 17 publications

References 10 publications

Measurement of H<sub>2</sub>S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

Measurement of H<sub>2</sub>S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

Application of the precolumn back‐flush technology in pesticide residue analysis: A practical view

Rapid determination of pesticide residues in herbs using selective pressurized liquid extraction and fast gas chromatography coupled with mass spectrometry

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