Kuklenyik Zsuzsanna, Ye Xiaoyun, Reich John Adam, Needham Larry L, Calafat Antonia M
Division of Laboratory Sciences, National Center for Environmental Health, Centers for Disease Control and Prevention, Atlanta, GA 30341, USA.
J Chromatogr Sci. 2004 Oct;42(9):495-500. doi: 10.1093/chromsci/42.9.495.
Automated online and off-line solid-phase extraction (SPE) methods coupled to isotope dilution-high-performance liquid chromatography-tandem mass spectrometry for measuring four isoflavones (daidzein, genistein, equol, and O-desmethylangolensin) and two lignans (enterolactone and enterodiol) in urine are developed. The SPE recoveries for the online SPE method are excellent for most analytes (83-94%) and somewhat lower for enterolactone (61%). The recoveries for all analytes with the off-line SPE method are also very good (65-80%). The limit of detection is lower for the online method (0.1-0.7 ng/mL) than for the off-line method (0.4-3.3 ng/mL). Similarly, the reproducibility is generally better for the online method [coefficient of variation (CV) of 4-12%) than for the off-line method, except for enterolactone, which has a higher CV (18-19%) that is consistent with its lower online SPE recovery. Both methods are adequate for analyzing a large number of samples for epidemiological studies to assess the prevalence of human exposure to isoflavones and lignans.
开发了在线和离线自动固相萃取（SPE）方法，结合同位素稀释-高效液相色谱-串联质谱法，用于测定尿液中的四种异黄酮（大豆苷元、染料木黄酮、雌马酚和O-去甲基安哥拉紫檀素）和两种木脂素（肠内酯和肠二醇）。在线SPE方法对大多数分析物的回收率极佳（83%-94%），而肠内酯的回收率略低（61%）。离线SPE方法对所有分析物的回收率也非常好（65%-80%）。在线方法的检测限（0.1-0.7 ng/mL）低于离线方法（0.4-3.3 ng/mL）。同样，除肠内酯外，在线方法的重现性通常优于离线方法[变异系数（CV）为4%-12%]，肠内酯的CV较高（18%-19%），这与其较低的在线SPE回收率一致。这两种方法都适用于分析大量样本，以进行流行病学研究，评估人类接触异黄酮和木脂素的流行情况。
