Fan Sai, Zou Jianhong, Xue Ying, Liu Ping, Wu Guohua, Zhao Rong
Beijing Centre for Disease Control and Prevention, Beijing 100013, China.
Wei Sheng Yan Jiu. 2017 Mar;46(2):309-317.
A method for determination of phthalate esters and their metabolites in blood by using SPE-ultra performance liquid chromatography tandem mass spectrometry.
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.
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%.
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.
建立一种利用固相萃取-超高效液相色谱串联质谱法测定血液中邻苯二甲酸酯及其代谢物的方法。
建立了一种稳定同位素检测方法，采用超高效液相色谱-质谱联用（UPLC-MS）结合固相萃取柱净化技术，测定血液中20种邻苯二甲酸酯及其6种代谢物。血样用乙酸盐缓冲液（pH5.2）稀释，经β-葡萄糖醛酸酶酶解12小时，然后用HLB柱净化。采用ACQUITY BEH苯基柱（2.1mm×100mm，1.7μm），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。本研究采用电喷雾电离（ESI）源，内标法定量。
26种分析物的线性范围为1.0 - 20.0μg/L，相关系数大于0.995。26种分析物的检测限均低于1.0μg/L。对添加了26种分析物、浓度分别为2.5、5.0和10.0μg/L的血清样品进行回收率研究，回收率在63.0% - 97.7%之间，相对标准偏差（RSD）为1.9% - 19.1%。
所建立的方法准确、灵敏，可用于血样中邻苯二甲酸酯及其代谢物残留的定性和定量分析。
