Improved HPLC Method Using 2,3-naphthalenedicarboxaldehyde as Fluorescent Labeling Agent for Quantification of Histamine in Human Immunoglobulin Preparations

Abstract

ObjectivesTo develop and optimize quantitative HPLC method using 2,3-naphthalenedicarboxaldehyde (NDA) after simple and efficient solid phase extraction to determine the histamine in a biopharmaceutical (Histobulin™).MethodsThe HPLC method was established using NDA-induced Histobulin and compared with the recently reported HPLC method using o-phthaldehyde (OPA). The validated NDA-applied HPLC method was adjusted to 15 lots of Histobulin and compared by the current lot-release-test method using fluorimetry in recovery of histamine and reproducibility.ResultsAnalyses of six HPLC chromatograms using NDA and OPA each were compared. NDA produced a more stable chromatogram baseline than OPA, and showed better stability. The HPLC analysis was validated in accuracy (91–103%), precision (interday/intraday assay CV ≤2.30%), and linearity of dose–response curve (R2 ≥ 0.9919). The detection limit was 0.0076 μg/mL and the quantitative limit was 0.0229 μg/mL. The amount of histamine per 12 mg of immunoglobulin was determined to be 0.17 ± 0.016 μg by the HPLC and 0.025 ± 0.013 μg by the current lot-release-test method using fluorimetry.ConclusionNDA derivatization showed better stability compared with the OPA method. Therefore the newly established NDA-derivatizated HPLC method may be more suitable than the fluorimetric method in lot-release-tests of biopharmaceuticals.

Development of a Rapid and Eco-Friendly UHPLC Analytical Method for the Detection of Histamine in Fish Products

“…Nevertheless, the proportion of the organic mobile phase of the method proposed was reduced to a minimum (15%) to reduce the environmental impact and the costs of each analysis. The quantity of organic solvent used is lower than other methods reported in the literature [ 55 , 56 ]; this modification did not compromise the separation of histamine during the analysis. Acetonitrile is not a green solvent according to the GAC approach [ 57 ] due to irritation, air hazard, and acute toxicity [ 58 ].…”

Novel approaches for the determination of biogenic amines in food samples

“…In the absence of other literature studies performed on wines, this reaction time was compared with other studies using NDA for BAs derivatization, observing that about 16 h are required to complete derivatization e.g. in human immunoglobulin samples [17]. This study, tests were performed at reaction times as long as16 h, highlighted a 30% decrease of the responses, probably due to degradation of the derivatizing products.…”

“…Studies involving BAs derivatization with NDA in biological human samples point out that concentration of 8·10 -5 M NDA was used to derivatize up to 0.15 mg/L (corresponding to 8·10 -7 M) histamine dihydrochloride [17]. Concentration of BAs in wines can achieve tens of mg/L.…”

“…Previous published works reported that NDA could be dissolved both in acetonitrile or methanol, without detailing if a contribution of the solvent in the derivatizing reaction is present [17,32].…”

Amperometric Biosensor Based on Diamine Oxidase/Platinum Nanoparticles/Graphene/Chitosan Modified Screen-Printed Carbon Electrode for Histamine Detection

“…Therefore, it is essential to implement fast, sensitive, selective and economical methods for the detection and quantification of histamine. These methods could be alternative or complementary to the classical methods, which principally consist of chromatography, for instance high performance liquid chromatography [ 12 ], cation-exchange chromatography [ 13 ], gas chromatography [ 14 ] or thin layer chromatography [ 15 ]. Detection of BAs by chromatographic methods requires derivation stage, pre- or post-column, to improve BA detection in ultraviolet, increasing the time of analysis and its cost.…”