Beljaars P R, Van Dijk R, Jonker K M, Schout L J
Inspectorate for Health Protection, Food Inspection Service, GA, Maastricht, The Netherlands.
J AOAC Int. 1998 Sep-Oct;81(5):991-8.
An interlaboratory study of the liquid chromatographic (LC) determination of histamine in fish, sauerkraut, and wine was conducted. Diminuted and homogenized samples were suspended in water followed by clarification of extracts with perchloric acid, filtration, and dilution with water. After LC separation on a reversed-phase C18 column with phosphate buffer (pH 3.0)--acetonitrile (875 + 125, v/v) as mobile phase, histamine was measured fluorometrically (excitation, 340 nm; emission, 455 nm) in samples and standards after postcolumn derivatization with o-phthaldialdehyde (OPA). Fourteen samples (including 6 blind duplicates and 1 split level) containing histamine at about 10-400 mg/kg or mg/L were analyzed singly according to the proposed procedure by 11 laboratories. Results from one participant were excluded from statistical analysis. For all samples analyzed, repeatability relative standard deviations varied from 2.1 to 5.6%, and reproducibility relative standard deviations ranged from 2.2 to 7.1%. Averaged recoveries of histamine for this concentration range varied from 94 to 100%.
开展了一项关于液相色谱法（LC）测定鱼类、酸菜和葡萄酒中组胺含量的实验室间研究。将切碎并均质化的样品悬浮于水中，然后用高氯酸澄清提取物，过滤并用水稀释。在以磷酸盐缓冲液（pH 3.0）-乙腈（875 + 125，v/v）为流动相的反相C18柱上进行LC分离后，用邻苯二甲醛（OPA）进行柱后衍生化，然后对样品和标准品进行荧光测定（激发波长340 nm；发射波长455 nm）。11个实验室按照所提议的程序单独分析了14个样品（包括6个盲样复制品和1个分割水平样品），这些样品中组胺含量约为10 - 400 mg/kg或mg/L。将一名参与者的结果排除在统计分析之外。对于所有分析的样品，重复性相对标准偏差在2.1%至5.6%之间，再现性相对标准偏差在2.2%至7.1%之间。该浓度范围内组胺的平均回收率在94%至100%之间。
