【摘要】 目的建立固相萃取-超高效液相色谱-串联三重四级杆质谱(UPLC-MS/MS)测定血液中20种邻苯二甲酸酯及其6种代谢产物的稳定同位素检测技术。方法血液样品经pH 5.2的乙酸钠缓冲盐稀释后,加入β-葡萄糖醛酸酶37℃下酶解12 h,经HLB固相萃取柱净化。在ACQUITYBEH Phenyl色谱柱(2.1 mm×100 mm,1.7μm)上以乙腈和含0.02%甲酸的水溶液为流动相进行梯度洗脱分离,采用ESI源模式进行二级子离子监测,内标法定量。结果 26种化合物的线性范围为1.0~20.0μg/L,相关系数(r)>0.995;各化合物检出限均低于1.0μg/L。以2.5、5.0和10.0μg/L为添加水平的血液的加标回收率为63.0%~97.7%,相对标准偏差为1.9%~19.1%。结论 UPLC-MS/MS法准确可靠,灵敏度高,可用于血液样品中邻苯二甲酸酯类化合物及其代谢产物残留的确证定性、定量检测。更多还原

【Abstract】 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.更多还原