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[Detection method of phthalate esters and their metabolites in blood]
Sai Fan1, Jianhong Zou1, Ying Xue1
1Beijing Centre for Disease Control and Prevention, Beijing 100013, China.
Objective:
A method for determination of phthalate esters and their metabolites in blood by using SPE-ultra performance liquid chromatography tandem mass spectrometry.
Methods:
A stable isotope detection method been developed for the determination of 20 kinds of phthalate esters and 6 kinds of phthalate esters metabolites in blood by ultra-performance liquid chromatography-mass spectrometry( UPLC-MS) coupled with SPE column purification. Blood samples were diluted with acetate buffer( pH5. 2), enzymatic hydrolyzed by β-glucuronidase for 12 h, then purified with HLB column. An ACQUITYBEH Phenyl column( 2. 1 mm ×100 mm, 1. 7 μm) was used for separation by the gradient elution with acetonitrile and aqueous solution containing 0. 02% formic acid as the mobile phases. In the present study, an electrospray ionization( ESI) source was used, and the internal standard method was used for quantitation.
Results:
The linear ranges of the 26 analytes were from 1. 0- 20. 0 μg/L, the coefficients of correlation were greater than 0. 995. The limits of detection( LODs) of the 26 analytes were all lower than1. 0 μg/L. Recoveries studies were carried out using serum samples fortified with the 26 analytes at the levels of 2. 5, 5. 0 and 10. 0 μg/L, recoveries were obtained in the range of63. 0%- 97. 7% with relative standard deviations( RSDs) from 1. 9% to 19. 1%.
Conclusion:
The established method is accurate and highly sensitive, and can be used for the qualitative and quantitative analysis of the residues of the phthalate esters and their metabolites in the blood samples.
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