色谱法
化学
邻苯二甲酸盐
串联质谱法
电喷雾电离
质谱法
固相萃取
检出限
酶水解
萃取(化学)
高效液相色谱法
液相色谱-质谱法
水解
分析物
电喷雾
定量分析(化学)
血清
生物化学
有机化学
医学
内分泌学
作者
Kayoko Kato,Manori J. Silva,John W. Brock,John A. Reidy,Nicole A. Malek,Carolyn C. Hodge,Hiroyuki Nakazawa,Larry L. Needham,Dana Boyd Barr
摘要
We developed a highly sensitive method for the quantitative detection of nine phthalate ester metabolites in human serum. This method requires denaturation of the serum enzymes immediately after blood collection to avoid the hydrolysis of the contaminant diester parent compounds introduced during blood collection and storage. Before analysis, the samples were subjected to an enzymatic deconjugation to hydrolyze the glucuronidated phthalate monoesters and a solid-phase extraction to isolate the monoesters from other serum components. The extracts were analyzed using reversed-phase high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry. The limits of detection of all nine phthalate monoesters in serum were in the low nanogram-per-milliliter range (0.6-1.3 ng/mL). Stable isotope-labeled internal standards for all analytes were used to improve precision and for recovery corrections. This highly selective method permits the analysis of phthalate monoesters without interferences resulting from the hydrolysis of the ubiquitous contaminant phthalate diesters by serum enzymes. In addition, it allows the direct measurement of the active phthalate monoester metabolites reportedly responsible for the reproductive and developmental toxicity of certain phthalates.
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