Analysis of histamine and N tau-methylhistamine in plasma by gas chromatography-negative ion-chemical ionization mass spectrometry.
Analysis of histamine and N tau-methylhistamine in plasma by gas chromatography-negative ion-chemical ionization mass spectrometry.
复制标题
采用气相色谱-负离子-化学电离质谱法分析血浆中的组胺和N-tau-甲基组胺。
DOI：
10.1016/0003-2697(89)90663-5
复制
发表时间：
1989
影响因子：
2.9
通讯作者：
Gerber,JG
中科院分区：
文献类型：
--
作者：
Payne,NA;Zirrolli,JA;Gerber,JG
目前组胺及其主要代谢物Nτ-甲基组胺的定量方法不准确，且对血浆样品中存在的极低浓度不敏感。因此，一个准确和灵敏的方法定量血浆中已开发使用稳定同位素稀释分析与负离子化学电离质谱。对于组胺，在向2 ml血浆中加入[2 H4]组胺后，将血浆样品脱蛋白，提取到丁醇中，反萃取到HCl中，衍生为五氟苄基衍生物（CH 2C 6 F5）3-组胺，在硅胶柱上纯化，然后通过选择离子监测离子m/z 430 - 434的比率，用负离子化学电离质谱法定量。对于Nτ-甲基组胺，向2 ml血浆中加入Nτ-[2 H3]甲基组胺后，将血浆样品脱蛋白，提取至丁醇中，反萃取至HCl中，衍生为七氟丁酰基衍生物（C3 F7 CO2）2-Nτ-甲基组胺，在硅胶柱上纯化，然后用负离子化学电离质谱法通过离子M/Z 497500的选择离子监测进行定量。组胺含量测定的精密度为3.1%，准确度为95.5 ± 2.5%; Nτ-甲基组胺含量测定的精密度为1.9%，准确度为106.8 ± 1.9%。组胺和Nτ-甲基组胺的灵敏度下限分别为1 pg和6 pg。在三名正常志愿者中使用该测定法，组胺的血浆浓度为130、92和85 pg/ml，Nτ-甲基组胺的血浆浓度为229、228和216 pg/ml。该测定法提供了一种非常灵敏和准确的定量血浆样品中组胺和Nτ-甲基组胺的方法。
Current methods of quantitation of histamine and its major metabolite Nτ-methylhistamine are inaccurate and insensitive to the very low concentrations that exist in plasma samples. Therefore, an accurate and sensitive method for quantification in plasma has been developed using the stable isotope dilution assay with negative ion-chemical ionization mass spectrometry. For histamine, after the addition of [2H4]histamine to 2 ml of plasma, the plasma sample is deproteinized, extracted into butanol, back extracted into HCl, derivatized to the pentafluorobenzyl derivative (CH2C6F5)3-histamine, purified on silica gel columns, and then quantified with negative ion-chemical ionization mass spectrometry by selected ion monitoring of the ratio of ions m z 430 434 . For Nτ-methylhistamine, after the addition of Nτ-[2H3]methylhistamine to 2 ml of plasma, the plasma sample is deproteinized, extracted into butanol, back extracted into HCl, derivatized to the heptafluorobutyryl derivative (C3F7CO2)2-Nτ-methylhistamine, purified on silica gel columns, and then quantified with negative ion-chemical ionization mass spectrometry by selected ion monitoring of the ratio of ions m z 497 500 . The precision of the histamine assay is 3.1% and the accuracy is 95.5 ± 2.5% while the precision of the Nτ-methylhistamine assay is 1.9% and the accuracy is 106.8 ± 1.9%. The lower limits of sensitivity are 1 pg for histamine and 6 pg for Nτ-methylhistamine injected on column. Using the assay in three normal human volunteers, plasma concentrations of histamine were 130, 92, and 85 pg/ml, and of Nτ-methylhistamine were 229, 228, and 216 pg/ml. This assay provides a very sensitive and accurate method of quantitation of histamine and Nτ-methylhistamine in plasma samples.