Determination of 16 phthalate metabolites in urine using automated sample preparation and on-line preconcentration/high-performance liquid chromatography/tandem mass spectrometry
Determination of 16 phthalate metabolites in urine using automated sample preparation and on-line preconcentration/high-performance liquid chromatography/tandem mass spectrometry
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DOI：
10.1021/ac0481248
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发表时间：
2005-05-01
影响因子：
7.4
通讯作者：
Calafat, AM
中科院分区：
文献类型：
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作者：
Kato, K;Silva, MJ;Calafat, AM
建立了一种在线固相萃取(SPE)、同位素稀释-高效液相色谱/串联质谱仪(HPLC/MS/MS)和自动样品制备相结合的方法，同时测定人尿中16种邻苯二甲酸酯类代谢物。该方法需要硅基整体柱用于尿液中邻苯二甲酸酯代谢物的初始预浓缩，以及硅基常规分析柱用于感兴趣的分析物的色谱分离。该方法尿量少(L 100亩)，灵敏度高(检出限为0.11~0.9 ng/mL)，加标回收率接近100%，精密度(日内、日间变异系数均为10%)。该方法不是劳动密集型的，而且由于尿样的预处理是使用高效液相自动取样器自动执行的，因此涉及的样品处理最少，因此最大限度地减少了接触危险化学品的风险。该方法在添加、混合的尿样和43名未接触邻苯二甲酸盐的成年人的尿样上得到验证。这种分析方法的高灵敏度和高通量(高效液相色谱运行时间，包括预浓缩步骤，为27分钟)，加上易于使用和有效的自动化样品制备程序，使其适合于大型流行病学研究，以评估人类接触邻苯二甲酸酯的流行率。
We developed an on-line solid-phase extraction (SPE) method, coupled with isotope dilution high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) and with automated sample preparation, to simultaneously quantify 16 phthalate metabolites in human urine. The method requires a silica-based monolithic column for the initial preconcentration of the phthalate metabolites from the urine and a silica-based conventional analytical column for the chromatographic separation of the analytes of interest. It uses small amounts of urine (100 mu L), is sensitive (limits of detection range from 0.11 to 0.90 ng/mL), accurate (spiked recoveries are similar to 100%), and precise (the inter- and intraday coefficients of variation are < 10%). The method is not labor intensive, and, because pretreatment of the urine samples was performed automatically using an HPLC autosampler, involves minimal sample handling, thus minimizing exposure to hazardous chemicals. The method was validated on spiked, pooled urine samples and on urine samples from 43 adults with no known exposure to phthalates. The high sensitivity and high throughput (HPLC run time, including the preconcentration step, is 27 min) of this analytical method combined with the ease of use and effective automated sample preparation procedure make it suitable for large epidemiological studies to evaluate the prevalence of human exposure to phthalates.