Quantitative detection of eight phthalate metabolites in human urine using HPLC-APCI-MS/MS
Quantitative detection of eight phthalate metabolites in human urine using HPLC-APCI-MS/MS
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DOI：
10.1021/ac000422r
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发表时间：
2000-09-01
影响因子：
7.4
通讯作者：
Brock, JW
中科院分区：
文献类型：
--
作者：
Blount, BC;Milgram, KE;Brock, JW
由于邻苯二甲酸酯的普遍存在及其在增加癌症和生殖功能障碍风险方面的潜在作用，迫切需要进行人体暴露评估研究。为了满足这一需求，我们开发了一种高通量、稳健、灵敏、准确和精确的检测方法，通过HPLC-MS/MS同时测量人尿液中八种邻苯二甲酸酯代谢物的痕量水平。使用酶解葡萄糖醛酸苷处理人尿液样本，然后进行固相萃取。浓缩邻苯二甲酸酯，通过反相HPLC色谱分离邻苯二甲酸酯代谢物，通过APCI串联质谱法检测，并通过同位素稀释定量。这种选择性的分析方法允许快速检测（总运行时间为7.7分钟）的八种最常用的邻苯二甲酸酯的尿液代谢物的检测限在低纳克每毫升范围。通过为八种分析物中的每一种加入C-13（4）标记的内标物以及结合的内标物以监测解结合效率，提高了测定精密度。这种选择性、灵敏和快速的方法将有助于阐明人体暴露于邻苯二甲酸酯与不良健康影响之间的潜在关联（如果有的话）。
Because of the ubiquity of phthalates and their potential role in increasing risk for cancer and reproductive dysfunction, the need for human exposure assessment studies is urgent. In response to this need, we developed a high-throughput, robust, sensitive, accurate, and precise assay for simultaneous measurement of trace levels of eight phthalate metabolites in human urine by HPLC-MS/MS. Human urine samples were processed using enzymatic deconjugation of the glucuronides followed by solid-phase ex-traction. The eluate was concentrated, and the phthalate metabolites were chromatographically resolved by reversed-phase HPLC, detected by APCI-tandem mass spectrometry, and quantified by isotope dilution. This selective analytical method permits rapid detection (7.7 min total run time) of eight urinary metabolites of the most commonly used phthalates with detection limits in the low nanagram per milliliter range. Assay precision Was improved by incorporating C-13(4)-labeled internal standards for each of the eight analytes, as well as a conjugated internal standard to monitor deconjugation efficiency. This selective, sensitive, and rapid method will help elucidate potential associations (if any) between human exposure to phthalates and adverse health effects.