Development of large volume injection method for capillary GC.

Tajima, Haruhiko; Shimamura, Naomi; Aoki, Masato

doi:10.2116/bunsekikagaku.42.10_573

Cited by 2 publications

(4 citation statements)

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“…Also, several applications of the LVI techniques for the analysis of pesticides have been reported; [3][4][5][6][7] however, there are few applications to dioxin analysis. [8][9][10][11] The representative LVI methods were a programmable temperature vaporizing (PTV) injection method [12][13][14] and a largevolume on-column injection method. 15,16 Also, other available methods were loop-type, 17,18 vapor-overflow 19,20 and concurrent solvent recondensation (CSR) 21 techniques.…”

Section: Introductionmentioning

confidence: 99%

Application of a Novel Large-Volume Injection Method Using a Stomach-Shaped Inlet Liner in Capillary Gas Chromatographic Trace Analysis of Dioxins in Human Milk and Plasma

et al. 2007

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A newly developed large-volume injection (LVI) technique that employs a unique stomach-shaped inlet liner (SSIL) inside of a programmable temperature vaporizer was used for the determination of trace amounts of dioxins in human milk and plasma. The initial temperature and the initial dwelling time of the inlet and the kind of solvent used were found to be critical in determining the analytical sensitivity of dioxins due to the loss of these relatively volatile compounds during solvent vaporization. Human milk and plasma were purified and fractionated by pre-packed multi-layered silicagel chromatography and activated carbon silica-gel column chromatography. A 20-μL aliquot of the fraction collected from the chromatography with toluene was directly applied to the LVI system in high-resolution gas chromatography/high-resolution mass spectrometry. Excellent correlation (r > 0.97) between the values obtained by the LVI method using the SSIL device and those by the conventional regular-volume splitless injection method was obtained for PCDDs, PCDFs and non-ortho PCBs in human milk and plasma samples.

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Section: Introductionmentioning

confidence: 99%

Application of a Novel Large-Volume Injection Method Using a Stomach-Shaped Inlet Liner in Capillary Gas Chromatographic Trace Analysis of Dioxins in Human Milk and Plasma

et al. 2007

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“…Some dioxin congeners in these samples, however, are present in concentrations below 1−2 pg/g lipid − and, hence, cannot be satisfactorily measured when several microliters of sample is injected into a HRGC/HRMS system. To improve the ability to detect dioxins, alternative methods employing enrichment techniques have been developed. − The AT column method (concentration at the inlet of the GC capillary precolumn for large-volume injection method) , has been found to increase both the sensitivity and detectability of dioxins. This method can also reduce the loss of relatively volatile dioxins, and the concentration/injection conditions are not as complex as those associated with solvent-cut large-volume injections (SCLV). − We show here an attempt to apply this technique to the introduction of sample volumes of up to 100 μL into HRGC/HRMS for separation/analysis of dioxins in blood.…”

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confidence: 99%

“…To improve the ability to detect dioxins, alternative methods employing enrichment techniques have been developed. [15][16][17][18][19][20][21] The AT column method (concentration at the inlet of the GC capillary precolumn for large-volume injection method) 22,23 to increase both the sensitivity and detectability of dioxins. This method can also reduce the loss of relatively volatile dioxins, and the concentration/injection conditions are not as complex as those associated with solvent-cut large-volume injections (SCLV).…”

mentioning

confidence: 99%

“…This method can also reduce the loss of relatively volatile dioxins, and the concentration/injection conditions are not as complex as those associated with solvent-cut large-volume injections (SCLV). [15][16][17][18][19][20][21] We show here an attempt to apply this technique to the introduction of sample volumes of up to 100 µL into HRGC/HRMS for separation/analysis of dioxins in blood.…”

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Development of a Method for Dioxin Analysis of Small Serum Samples with Reduced Risk of Volatilization

et al. 2005

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To analyze the dioxin content of samples, including dibenzo-p-dioxins/dibenzofurans, and coplanar polychlorinated biphenyls (Co-PCBs), a large volume is usually necessary. This is difficult, however, when analyzing clinical samples, such as serum and tissue. We therefore sought to increase the sensitivity of high-resolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS) in analyzing dioxins by injecting most of the extract from a small clinical sample. The concentration of each congener was estimated by injecting extracts of 5-g samples into a gas chromatography capillary precolumn (AT column) and by assaying extracts of 25-g samples by conventional splitless methods. We found that the limit of detection with the AT column was lower than that obtained by the splitless technique. In the AT column technique, 100 microL of the 110-microL final solution, equivalent to 4.5 g of the original sample, was injected into HRGC/HRMS. In contrast, 2 microL of the 20-microL final solution, equivalent to 2.5 g of original sample, was assayed using the splitless method. Moreover, when 25 fg of ultratrace dioxin was added to 100 microL of HRGC/HRMS sample and injected into the AT column, the peak area was almost the same as that obtained with 2 microL of HRGC/HRMS sample injected using the splitless method. Although assaying 10-20 microL of sample by the splitless method presents difficulties due to sample volatility, this problem can be reduced by using volumes larger than 100 microL. We tested this application by quantifying the parts-per-trillion levels, on a lipid weight basis, of each congener in a serum sample of 5 g using the AT column HRGC/HRMS method. We found this application to be successful and practical for mass screening of dioxin exposure in clinical samples.

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Development of large volume injection method for capillary GC.

Cited by 2 publications

References 0 publications

Application of a Novel Large-Volume Injection Method Using a Stomach-Shaped Inlet Liner in Capillary Gas Chromatographic Trace Analysis of Dioxins in Human Milk and Plasma

Application of a Novel Large-Volume Injection Method Using a Stomach-Shaped Inlet Liner in Capillary Gas Chromatographic Trace Analysis of Dioxins in Human Milk and Plasma

Development of a Method for Dioxin Analysis of Small Serum Samples with Reduced Risk of Volatilization

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