An immunoglobulin (IgG) preparation with micro-amount of histamine fixed on the active protein fraction has been used to increase the resistance to allergic reactions. However, excessive histamine may cause hypo- or hypertension, headache, or anaphylactic shock and so the histamine content of the drug is strictly controlled by a regulation: 0.15 μg of histamine dihydrochloride is allowed for 12 mg of immunoglobulin. In this study, a liquid Chromatographic method to determine micro-amount of histamine in the pharmaceutical was developed and validated. This method include a sample cleanup by a solid phase extraction (SPE) using a polystyrenedivinyl benzene (PS-DVB) polymeric sorbent and high-performance liquid chromatography after precolumn fluorescent labeling of the histamine with o-phthaldialdehyde. The drug sample was loaded to the SPE cartridge after adjusting to pH 9.5. After successive washings of the cartridge with water and 30% aqueous methanol, histamine was then eluted with 100 mM sodium acetate (pH 9.5)-methanol (20:80, v/v). An aliquot from the eluate was labeled with o-phthaldialdehyde-mercaptoethanol (OPA-ME) for fluorescence detection at the excitation maximum of 340 nm and emission maximum of 450 nm. HPLC analysis was performed on a phenyl-hexyl column with an acetonitrile-phosphate buffer (pH 6.8; 50 μM) (35:65, v/v) as the mobile phase. The retention times of histamine and 3-methylhistamine (IS) were approximately 7.2 and 9.5 min, respectively. The quantitation range was between 0.01-0.2 mg/mL of histamine showing good linearity (r=0.9996). This analytical method would provide a potential mean for the strict control of histamine content in the pharmaceutical product.
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Armagan, O., Current analytical methods for the determination of biogenic amines in foods.Food Chemistry, 103, 1475–1486 (2007).
Ayoub, M., Mittenbuhler, K., Sutterlin, B. W., and Bessler, W. G, The anti-allergic drug histaglobin inhibits NF-kappaB nuclear translocation and down-regulates proinflammatory cytokines.Int. J. Immunopharmacol., 22, 755–763 (2000).
Busto, O., Guasch, J., and Borrul, R, Biogenic amines in wine: A review of analytical methods.J. Int.Sci.Vigne. Vin., 30, 85- 101 (1996).
Gilbert, R. J., Hobbes, G, Murray, C. K., Cruickshank, J. G, and Young, S. E., Scombrotoxic fish poisoning: feature of the first 50 incidents to be reported in Britain (1976’9).Br. Med J., 281, 71–72 (1980).
George, J. S., Michelle, C, and David, M. G, Method development and cultivar-related differences of nine biogenic amines in Ontario wines.Food Chemistry, 64, 49–58 (1999).
Gushchin, I. S., Luss, L V, Nina, N. I., Larina, O. N., and Pakhomova, L. A., Therapeutic activeness of histaglobin preparations in patients with allergic rhinitis and chronic urticaria.Ter. Arkh., 71, 57–62 (1999).
Ishikawa, T, Shimada, T, Kessoku, N., and Kiyoi, M., Inhibition of rat mast cell degranulation and histamine release by histamine-rat gamma-globulin conjugate.Int. Arch. Allergy. Appl. Immunol., 59, 403–407 (1979).
Liebhart, J., Zak-Najmark, T, Malolepszy, J., Nadobna, G, and Liebhart, E., Changes of histaminopexy in patients with bronchial asthma and chronic urticaria after histaglobin administration.Arch. Immunol. Ther. Exp. (Warsz), 34, 385- 389 (1986).
Maurizio, P., Andrea, R., Lucia, B., Alina, P., Debora, B., Cristina, V, Irene, L., Elisa, C, Massimo, S., Francesco, F., Blo G and Capitani S., Determination of histamine in the whole blood of colon cancer patients.J. Chromatogr. B., 780, 331–339 (2002).
May, S., Sturman, G, and Perrett, D., Determination of histamine in tissues using reversed phase-HPLC with post column fluorimetric detection.Inflamm. Res., 48, S94–95 (1999).
Molins-Legua, C, Campins-Falco, P., and Sevillano-Cabeza, A., Automated pre-column derivatization of amines in biological samples with dansyl chloride and with or without post-column chemiluminescence formation by using TCPO-H 2O2. Analyst., 123, 2871–2876 (1998).
Molins-Legua, C, Campins-Falco, P., and Sevillano-Cabeza, A., M. Pedron-Pons, Urine polyamines determination using dansyl chloride derivatization in solid-phase extraction cartridges and HPLC.Analyst, 124, 477–482 (2000).
Oguri, S. and Yoneya, Y, Selective detection of biogenic amines using capillary electrochromatography with an oncolumn derivatization technique.J. Chromatogr. B., 781, 165- 179 (2002).
Ohnishi, A., Watanabe, K., Nakagawa, T., Morita, Y, and Miyamoto, T, Inhibitory effect of histamine-added human gammaglobulin on histamine release from human leucocytes.Clin. Immunol., 17, 1145–1150 (1985).
Pad, A., Taddeucci-Brunelli, G, Barachini, P., Magliaccio, P., Pierini, G, and Crimaldi, G, Therapy of atopic dermatitis in childern. Study on the use of a desensitizing preparation.Pediatr. Med. Chir, 8, 839–844 (1986).
Parrot, J. L. and Laborde, C, The histamine-fixing power of blood serum; its modification after an injection of normal human serum or of an azoprotein of histamine.J. Physiol. (Paris), 46, 492–495 (1954).
Paul, R. B., Van Dijk, Remmelt, Klaas, M. J., and Louis J. S., Liquid Chromatographic Determination of Histamine in Fish, Sauerkraut, and Wine Interlaboratory Study.J. AOAC. Int., 81, 991–998 (1999).
Simon-Sarkadi, L. and Holzapfel, W. H. Z., Determination of biogenic amines in leafy vegetables by amino acid analyzer.Z. Lebensm. Unters. Forsch., 198, 230–233 (1994).
Taylor, S. L. and Speckhard, M. W., Inhibition of bacteria histamine production by sorbate and other antimicrobial agents.J. Food. Prot., 47, 508–511 (1984).
Taylor, S. L, Histamine food poisoning: Toxicology and clinical aspects.Crit. Rev. Toxicol., 17, 91–128 (1986).
Valeria, F. and Claudia, L, Histamine and histidine determination in tuna fish samples using high-performance liquid chromatography.J. Chromatogr. A., 809, 241–245 (1998).
Wollin, A., Soll, A. H., and Samloff, I. M., Actions of histamine, secretin, and PGE2 on cyclic AMP production by isolated canine fundic mucosal cells.Am. J. Physiol., 237, E437–443 (1979).
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Kim, N.H., Park, Y., Jeong, E.S. et al. A liquid chromatographic method for the determination of histamine in immunoglobulin preparation using solid phase extraction and pre-column derivatization. Arch. Pharm. Res. 30, 1350 (2007). https://doi.org/10.1007/BF02980277
- Immunoglobulin preparation
- Solid-phase extraction
- Fluorescent detection