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KMID : 0043320070300101350
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Archives of Pharmacal Research
2007 Volume.30 No. 10 p.1350 ~ p.1357
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A Liquid Chromatographic Method for the Determination of Histamine in Immunoglobulin Preparation Using Solid Phase Extraction and Pre-Column Derivatization
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Kim Nam-Hee
Park You-Mie
Jeong Eun-Sook
Kim Chang-Soo
Jeong Min-Kyo
Kim Kyoung-Soon
Hong Seung-Hwa
Son Jong-Keun
Hong Jin-Tae
Park Il-Young
Moon Dong-Cheul
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Abstract
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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 ophthaldialdehyde- 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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KEYWORD
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Immunoglobulin preparation, Histamine, Solid-phase extraction, PS-DVB, Fluorescent detection, o-Phthaldialdehyde
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