Modification of cleanup methods for dioxin analysis in green leafy vegetables and comparison of packing methods for a multi-layer silica gel column

To determine polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and coplanar polychlorinated biphenyls (Co-PCBs) in green leafy vegetables, the cleanup method was modified, and packing methods for a multi-layer silica gel column were compared in food samples. First, the...

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Published inFood Hygiene and Safety Science (Shokuhin Eiseigaku Zasshi) Vol. 44; no. 6; pp. 321 - 327
Main Authors Amakura, Y. (National Inst. of Hygienic Sciences, Tokyo (Japan)), Tsutsumi, T, Sasaki, K, Maitani, T
Format Journal Article
LanguageEnglish
Published Japan Japanese Society for Food Hygiene and Safety 01.12.2003
Subjects
ANALYTICAL METHODS
Chromatography, Gel - methods
cleanup
COLUMN CHROMATOGRAPHY
coplanar PCB
DIOXINS
Dioxins - analysis
Food Handling - methods
green leafy vegetable
LEAF VEGETABLES
multi-layer silica gel column
PCDD
PCDF
Spinacia oleracea - chemistry
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Abstract To determine polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and coplanar polychlorinated biphenyls (Co-PCBs) in green leafy vegetables, the cleanup method was modified, and packing methods for a multi-layer silica gel column were compared in food samples. First, the additional cleanup was examined for a mono-ortho PCBs fraction obtained by alumina column chromatography from spinach extract. Small solids such as rough crystals that remained after concentration of the mono-ortho PCBs fraction were identified as long-chain hydrocarbons from leaf epicuticular wax by GC/MS. Cleanup using an activated carbon silica gel column with n-hexane as the washing solvent was effective. Next, multi-layer silica gel columns packed by wet packing and dry packing were compared using komatsuna, salmon and butter as samples. The columns prepared by both methods gave similar values at each isomeric concentration level and showed similar efficiency with favorable recoveries.
AbstractList To determine polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and coplanar polychlorinated biphenyls (Co-PCBs) in green leafy vegetables, the cleanup method was modified, and packing methods for a multi-layer silica gel column were compared in food samples. First, the additional cleanup was examined for a mono-ortho PCBs fraction obtained by alumina column chromatography from spinach extract. Small solids such as rough crystals that remained after concentration of the mono-ortho PCBs fraction were identified as long-chain hydrocarbons from leaf epicuticular wax by GC/MS. Cleanup using an activated carbon silica gel column with n-hexane as the washing solvent was effective. Next, multi-layer silica gel columns packed by wet packing and dry packing were compared using komatsuna, salmon and butter as samples. The columns prepared by both methods gave similar values at each isomeric concentration level and showed similar efficiency with favorable recoveries.
To determine polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and coplanar polychlorinated biphenyls (Co-PCBs) in green leafy vegetables, the cleanup method was modified, and packing methods for a multi-layer silica gel column were compared in food samples. First, the additional cleanup was examined for a mono-ortho PCBs fraction obtained by alumina column chromatography from spinach extract. Small solids such as rough crystals that remained after concentration of the mono-ortho PCBs fraction were identified as long-chain hydrocarbons from leaf epicuticular wax by GC/MS. Cleanup using an activated carbon silica gel column with n-hexane as the washing solvent was effective. Next, multi-layer silica gel columns packed by wet packing and dry packing were compared using komatsuna, salmon and butter as samples. The columns prepared by both methods gave similar values at each isomeric concentration level and showed similar efficiency with favorable recoveries.To determine polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and coplanar polychlorinated biphenyls (Co-PCBs) in green leafy vegetables, the cleanup method was modified, and packing methods for a multi-layer silica gel column were compared in food samples. First, the additional cleanup was examined for a mono-ortho PCBs fraction obtained by alumina column chromatography from spinach extract. Small solids such as rough crystals that remained after concentration of the mono-ortho PCBs fraction were identified as long-chain hydrocarbons from leaf epicuticular wax by GC/MS. Cleanup using an activated carbon silica gel column with n-hexane as the washing solvent was effective. Next, multi-layer silica gel columns packed by wet packing and dry packing were compared using komatsuna, salmon and butter as samples. The columns prepared by both methods gave similar values at each isomeric concentration level and showed similar efficiency with favorable recoveries.
Author Maitani, T
Sasaki, K
Amakura, Y. (National Inst. of Hygienic Sciences, Tokyo (Japan))
Tsutsumi, T
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References 1) Shokuhinchu No Daiokishinrui Oyobi Kopurana PCB No Sokuteihouhou Zantei Gaidorain (Provisional guidelines for analysis of polychlorinated dibenzo-p-dioxins, dibenzofurans and coplanar PCBs in Foods) (Oct., 1999). Environmental Health Bureau, Ministry of Health and Welfare (Present name: Pharmaceutical and Food Safety Bureau, Ministry of Health, Labour and Welfare), Japan.
8) Hori, T., Nakagawa, R., Tobiishi, K., Iida, T., Tsutsumi, T., Sasaki, K., Toyoda, M., Effects of cooking on concentrations of polychlorinated dibenzo-p-dioxins and related compounds in green leafy vegetable 'Komatsuna'. Shokuhin Eiseigaku Zasshi (J. Food Hyg. Soc. Japan), 42, 339-342 (2001).
10) Grossi, V., Raphel, D., Long-chain (C19-C29) 1-chloro-n-alkanes in leaf waxes of halophytes of the Chenopodiaceae. Phytochemistry, 63, 693-698 (2003).
11) Maffei, M., Chemotaxonomic significance of leaf wax n-alkanes in the Umbelliferae, Cruciferae and Leguminosae (Subf. Papilionoideae). Biochem. Syst. Ecol., 24, 531-545 (1996).
6) Tsutsumi, T., Iida, T., Hori, T., Nakagawa, R., Tobiishi, K., Yanagi, T., Kono, Y., Uchibe, H., Matsuda, R., Sasaki, K., Toyoda, M., Recent survey and effects of cooking processes on levels of PCDDs, PCDFs and Co-PCBs in leafy vegetables in Japan. Chemosphere, 46, 1443-1449 (2002).
4) Amakura, Y., Tsutsumi, T., Sasaki, K., Toyoda, M., Maitani, T., Comparison of sulfuric acid treatment and multi-layer silica gel column chromatography in cleanup methods for determination of PCDDs, PCDFs and dioxin-like PCBs in foods. Shokuhin Eiseigaku Zasshi (J. Food Hyg. Soc. Japan), 43, 312-321 (2002).
7) Tsutsumi, T., Yanagi, T., Nakamura, M., Kono, Y., Uchibe, H., Iida, T., Hori, T., Nakagawa, R., Tobiishi, K., Matsuda, R., Sasaki, K., Toyoda, M., Update of daily intake of PCDDs, PCDFs, and dioxin-like PCBs from food in Japan. Chemosphere, 45, 1129-1137 (2001).
9) van den Berg, M., Birnbaum, L., Bosveld, A. T. C., Brunstrom, B., Cook, P., Feeley, M., Giesy, J. P., Hanberg, A., Hasegawa, R., Kennedy, S. W., Kubiak, T., Larsen, J. C., van Leeuwen, F. X. R., Liem, A. K. D., Nolt, C., Peterson, R. E., Poellinger, L., Safe, S., Schrenk, D., Tillitt, D., Tysklind, M., Younes, M., Warn, F., Zacharewski, T., Toxic equivalency factors (TEFs) for PCBs, PCDDs, PCDFs for humans and wildlife. Environmental Health Perspectives, 106, 775-792 (1998).
2) Amakura, Y., Tsutsumi, T., Sasaki, K., Toyoda, M., Maitani, T., Cleanup of food samples with pre-packed multi-layer silica gel column for the analysis of PCDDs, PCDFs and dioxin-like PCBs. Shokuhin Eiseigaku Zasshi (J. Food Hyg. Soc. Japan), 44, 119-125 (2003).
3) Tsutsumi, T., Amakura, Y., Sasaki, K., Toyoda, M., Maitani, T., Evaluation of an aqueous KOH digestion followed by hexane extraction for analysis of PCDD/Fs and dioxin-like PCBs in retailed fish, Anal. Bioanal. Chem., 375, 792-798 (2003).
5) Nakagawa, R., Hori, T., Tobiishi, K., Iida, T., Tsutsumi, T., Sasaki, K., Toyoda, M., Levels and tissue-dependent distribution of dioxin in Japanese domestic leafy vegetables—from the 1999 national investigation. Chemosphere, 48, 247-256 (2002).
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2
AMAKURA Y (4) 2002; 43
5
6
7
TSUTSUMI T (3) 2003; 375
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HORI T (8) 2001; 42
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References_xml – reference: 11) Maffei, M., Chemotaxonomic significance of leaf wax n-alkanes in the Umbelliferae, Cruciferae and Leguminosae (Subf. Papilionoideae). Biochem. Syst. Ecol., 24, 531-545 (1996).
– reference: 4) Amakura, Y., Tsutsumi, T., Sasaki, K., Toyoda, M., Maitani, T., Comparison of sulfuric acid treatment and multi-layer silica gel column chromatography in cleanup methods for determination of PCDDs, PCDFs and dioxin-like PCBs in foods. Shokuhin Eiseigaku Zasshi (J. Food Hyg. Soc. Japan), 43, 312-321 (2002).
– reference: 2) Amakura, Y., Tsutsumi, T., Sasaki, K., Toyoda, M., Maitani, T., Cleanup of food samples with pre-packed multi-layer silica gel column for the analysis of PCDDs, PCDFs and dioxin-like PCBs. Shokuhin Eiseigaku Zasshi (J. Food Hyg. Soc. Japan), 44, 119-125 (2003).
– reference: 5) Nakagawa, R., Hori, T., Tobiishi, K., Iida, T., Tsutsumi, T., Sasaki, K., Toyoda, M., Levels and tissue-dependent distribution of dioxin in Japanese domestic leafy vegetables—from the 1999 national investigation. Chemosphere, 48, 247-256 (2002).
– reference: 3) Tsutsumi, T., Amakura, Y., Sasaki, K., Toyoda, M., Maitani, T., Evaluation of an aqueous KOH digestion followed by hexane extraction for analysis of PCDD/Fs and dioxin-like PCBs in retailed fish, Anal. Bioanal. Chem., 375, 792-798 (2003).
– reference: 10) Grossi, V., Raphel, D., Long-chain (C19-C29) 1-chloro-n-alkanes in leaf waxes of halophytes of the Chenopodiaceae. Phytochemistry, 63, 693-698 (2003).
– reference: 1) Shokuhinchu No Daiokishinrui Oyobi Kopurana PCB No Sokuteihouhou Zantei Gaidorain (Provisional guidelines for analysis of polychlorinated dibenzo-p-dioxins, dibenzofurans and coplanar PCBs in Foods) (Oct., 1999). Environmental Health Bureau, Ministry of Health and Welfare (Present name: Pharmaceutical and Food Safety Bureau, Ministry of Health, Labour and Welfare), Japan.
– reference: 6) Tsutsumi, T., Iida, T., Hori, T., Nakagawa, R., Tobiishi, K., Yanagi, T., Kono, Y., Uchibe, H., Matsuda, R., Sasaki, K., Toyoda, M., Recent survey and effects of cooking processes on levels of PCDDs, PCDFs and Co-PCBs in leafy vegetables in Japan. Chemosphere, 46, 1443-1449 (2002).
– reference: 7) Tsutsumi, T., Yanagi, T., Nakamura, M., Kono, Y., Uchibe, H., Iida, T., Hori, T., Nakagawa, R., Tobiishi, K., Matsuda, R., Sasaki, K., Toyoda, M., Update of daily intake of PCDDs, PCDFs, and dioxin-like PCBs from food in Japan. Chemosphere, 45, 1129-1137 (2001).
– reference: 8) Hori, T., Nakagawa, R., Tobiishi, K., Iida, T., Tsutsumi, T., Sasaki, K., Toyoda, M., Effects of cooking on concentrations of polychlorinated dibenzo-p-dioxins and related compounds in green leafy vegetable 'Komatsuna'. Shokuhin Eiseigaku Zasshi (J. Food Hyg. Soc. Japan), 42, 339-342 (2001).
– reference: 9) van den Berg, M., Birnbaum, L., Bosveld, A. T. C., Brunstrom, B., Cook, P., Feeley, M., Giesy, J. P., Hanberg, A., Hasegawa, R., Kennedy, S. W., Kubiak, T., Larsen, J. C., van Leeuwen, F. X. R., Liem, A. K. D., Nolt, C., Peterson, R. E., Poellinger, L., Safe, S., Schrenk, D., Tillitt, D., Tysklind, M., Younes, M., Warn, F., Zacharewski, T., Toxic equivalency factors (TEFs) for PCBs, PCDDs, PCDFs for humans and wildlife. Environmental Health Perspectives, 106, 775-792 (1998).
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  issn: 0015-6426
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  doi: 10.1016/S0031-9422(03)00283-8
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  doi: 10.3358/shokueishi.43.312
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Snippet To determine polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and coplanar polychlorinated biphenyls (Co-PCBs) in green leafy...
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SubjectTerms ANALYTICAL METHODS
Chromatography, Gel - methods
cleanup
COLUMN CHROMATOGRAPHY
coplanar PCB
DIOXINS
Dioxins - analysis
Food Handling - methods
green leafy vegetable
LEAF VEGETABLES
multi-layer silica gel column
PCDD
PCDF
Spinacia oleracea - chemistry
Title Modification of cleanup methods for dioxin analysis in green leafy vegetables and comparison of packing methods for a multi-layer silica gel column
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