Survey of Histamine Content in Seafood on the Market

Transcription

1 June , Survey of Histamine Content in Seafood on the Market Kimiko K6C,Hirofumi UH=>N6B6, Tetsuya S=>C9D and Kazuo S6>ID (Tokyo Metropolitan Institute of Public Health: , Hyakunin-cho, Shinjuku-ku, Tokyo , Japan; Corresponding author) Food poisoning involving histamine has occurred almost every year for 20 years in Tokyo, and is usually due to ingestion of fish with lean meat, such as sardine, mackerel, horse mackerel and so on. Therefore, we were investigated the levels of histamine and 4 non-volatile amines (tyramine, putrescine, cadaverine, spermidine) in 637 samples on the market. The water activity of samples in which histamine was detected at 5 mg/100 g and over was examined. Histamine, tyramine, putrescine, cadaverine and spermidine were detected in 66, 43, 26, 64 and 5 samples, and the detection ranges were 5 340, 5 51, 5 42, and 5 8 mg/100 g, respectively. Most of the samples in which histamine was detected were semi-dried round and split sardine. Water activity of 24 samples of semi-dried round and split sardine in which histamine was detected was in the range of (Received December 16, 2004) Key words: histamine; non-volatile amine; survey; fish; big-eye sardine; water activity; seafood 1) 16) 20 17) 19) 13), 16), 20) 24) ) )

2 ) (99 ) 100 mg 0.5 mol/l 100 ml 1,000 mg/ml 100 mg/ml 0.5 mol/l 250 mg/ml 50 mg/ml 10 mg/ml 10 mg/ml 10 mg/ml 0.5 mol/l 2) 1,6-10 mg/ml 0.5 mol/ L 3. 1) (HPLC) LC-10 ATVP RF-10AXL, CTO-10 Vol. 46, No. 3 AVP SIL-10ADVP 2) AW-2 Hygroskop DT Rotronic 3) MOV-212 (U) 4. 17) (TLC) HPLC Scheme 1 5mg/100 g (TLC) Kieselgel 60 Merck 28 (9 : 1) I) 0.01 / 365 nm II) 0.1 / HPLC Inertsil ODS-80A (5 mm, 250 mm 4.6 mm i.d.) 40 (62 : 38) 1.5 L/min 325 nm 525 nm) 5. Sample 10 g add H 2 O15mL homogenize add 10 trichloroacetic acid solution 20 ml make up to 50 ml with water keep at room temp. for 10 min filter (No. 5A paper) Filtrate Test solution for TLC Sample solution Mixed standard solution (Qualitative analysis) 0.5 ml ml make up to 1 ml with water add internal standard 0.5 ml add Na 2 CO g add 1 dansyl chloride/acetone solution 1 ml stand at 45 in a waterbath (or at room temp. overnight) add 10 proline solution 0.5 ml stand for 10 min add toluene 5.0 ml shake Toluene layer evaporate Residue make up to 1.0 ml with acetonitrile Test solution for HPLC (Quantitative analysis) Scheme 1. Analytical procedure for non-volatile amines

3 June Table 1. Detection and Contents of Non-volatile Amines in Commercial Fish No. Fish Number of samples Detected (content: mg/100 g) Histamine Tyramine Putrescine Cadaverine Spermidine 1 Sardine (Iwashi-rui) (6 340) 38 (5 51) 23 (5 42) 60 (5 180) 5 (5 8) 2 Skipjack and frigate mackerel (Katsuo-rui) 32 6 (5 82) 5 (6 48) 1 (6) Horse mackerel (Aji-rui) (12, 30) (30) 0 4 Mackerel (Saba-rui) 35 2 (10, 10) Pacific saury (Sanma) 35 1 (16) (9) 0 6 Blue sprat (Kibinago) 4 1 (30) 0 2 (8, 10) 2 (16, 81) 0 7 Tuna (Maguro-rui) Marline and Swordfish (Kajiki-rui) Spanish mackerel (Sawara-rui) Shishamo Yellowtail (Buri-rui) Flying fish (Tobiuo-rui) Japanese sand lance (Ikanago) Pacific herring (Nishin) Atka mackerel (Hokke) Acropoma japonicum (Hotarujako) Gizzard shad (Konoshiro) Butterfish (Ibodai) Barracuda (Kamasu-rui) Big-eyed herring (Sappa) Dolphinfish (Shiira) Salmon (Sake-rui) Opah (Mandai) Total (5 340) 43 (5 51) 26 (5 42) 64 (5 180) 5 (5 8) Table 2. Detection and Contents of Non-volatile Amines in Processed Fish Products Form Number of samples Detected (content: mg/100 g) Histamine Tyramine Putrescine Cadaverine Spermidine Raw (Fresh) 73 1 (16) (9) 0 Seasoned raw (Ajitsuke nama) Semi-dried, round and split (Himono) (6 340) 35 (5 51) 25 (5 42) 60 (7 180) 5 (5 8) Seasoned and dried (Ajitsuke himono) Brine-soaked and dried (Kusaya) Boiled and dried whole (Niboshi) Boiled and dried whitebait (Shirasuboshi) Paste products (Neriseihin) 78 5 (7 34) 1 (23) 0 3 (5 70) 0 Pickled (Suzuke) Seasoned and boiled (Tsukudani) 11 1 (8) 1 (5) Boiled meat (Namari) Dried strip (Katsuobushi) Stock (Dashi) Seasoned powder for sprinkling (Furikake) 15 6 (5 82) 6 (5 48) 1 (6) 0 0 Canned (Kanzume) Salted viscera preserves (Shiokara) 3 1 (12) Total (5 340) 43 (5 51) 26 (5 42) 64 (5 180) 5 (5 8) 6. 5g Table 1 Table mg/100 g 69 mg/100 g 10

4 mg/100 g 17 mg/100 g mg/ 100 g 11 mg/100 g mg / 100 g 47 mg/100 g mg/100 g 6mg/100 g 5 1 1) mg/100 g 61 mg/100 g mg/100g 22 mg/100 g mg/100 g 21 mg/100 g mg/100 g mg/100 g mg/100 g 82 2) mg/100 g 82 mg/100 g mg / 100 g 22 mg/100 g mg/100 g 19 mg/100 g mg/100 g mg/100 g mg/100 g Vol. 46, No /3 17), 24) 100 mg/100 g Table g mg 24) 100 mg mg mg mg 3 5 3) Table 3. Water Activity and Water Content of Big-eye Sardine in which Histamine was Detected (Urume-iwashi, 100 mg/100 g and over) No. Sample Histamine concentration (mg/100 g) Weight (g) Histamine (mg)/fish Water activity Water content ( ) 1 Big-eye sardine Big-eye sardine Big-eye sardine Big-eye sardine Big-eye sardine Big-eye sardine Big-eye sardine Big-eye sardine Big-eye sardine Big-eye sardine Big-eye sardine Big-eye sardine Big-eye sardine Not tested, Salted and dried whole

5 June Fig. 1. Relationship of water activity and number of samples containing histamine (semi-dried, round and split sardine) ) 26) ) 29) 5 mg/100 g Fig ) 27) 3. Table mg/100 g mg/100 g mg/100 g (5 51 mg/100 g) (5 42 mg/ 100 g) (5 180 mg/100 g) (5 8 mg/100 g) 100 mg 1) Maki, T., Kan, K., Nagayama, T., Iida, M., Nishima, T., Outbreaks of food poisoning of chemical and naturally occurring toxicants in Tokyo (III) (1985). Tokyo 37, (1986). 2) Maki, T., Kan, K., Nagayama, T., Iida, M., Nishima, T., Outbreaks of food poisoning of chemical and naturally occurring toxicants in Tokyo (IV) Tokyo 38, (1987). 3) Maki, T., Kan, K., Nagayama, T., Iida, M., Kawai, Y., Nishima, T., Outbreaks of food poisoning of chemical and naturally occurring toxicants in Tokyo (V) Tokyo Eiken Nenpo (Ann. Rep. Tokyo Metr. Res. Lab. P.H.), 39, (1988). 4) Maki, T., Kan, K., Nagayama, T., Iida, M., Kawai, Y., Nishima, T., Outbreaks of food poisoning of chemical and naturally occurring toxicants in Tokyo (VI) Tokyo Eiken Nenpo (Ann. Rep. Tokyo Metr. Res. Lab. P.H.), 40, (1989). 5) Maki, T., Kan, K., Nagayama, T., Hashimoto, H., Kawai, Y., Iida, M., Kobayashi, M., Shioda, H., Nishima, T., Outbreaks toxicants in Tokyo (VII) Tokyo 41, (1990). 6) Maki, T., Kan, K., Hashimoto, H., Nishima, T., Outbreaks toxicants in Tokyo (IX) Tokyo Eiken Nenpo (Ann. Rep. Tokyo Metr. Res. Lab. P. H.), 43, (1992).

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