超高效液相色谱串联三重四极杆质谱法快速测定人血清中双酚A和4-叔丁基苯酚  

Rapid determination of bisphenol A and 4-tert-butylphenol in human serum by ultra-performance liquid chromatography coupled to tandem triple quadrupole mass spectrometry

作　　者：朱传新[1] 郑艳容[1] 

机构地区：[1]温州市疾病预防控制中心,浙江温州325001

出　　处：《中国卫生检验杂志》2016年第12期1689-1692,共4页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立人血清中双酚A(BPA)和4-叔丁基苯酚(4-t-BP)的超高效液相色谱串联三重四极杆质谱测定方法。方法取200μl血清用β-葡萄糖醛酸酶水解,甲基叔丁基醚萃取,丹酰氯衍生化后,采用C18超高效液相色谱柱和含0.1%甲酸的甲醇和水流动相梯度洗脱分离,三重四极杆质谱仪测定,内标标准曲线法定量。结果 BPA和4-t-BP浓度为0.1 ng/ml^50 ng/ml时,线性关系良好,相关系数(r)均>0.995;3倍基线噪声所对应的BPA、4-t-BP的方法检出限分别为0.05 ng/ml和0.07 ng/ml。在1.0 ng/ml、2.0 ng/ml和10 ng/ml 3种加标水平下,BPA和4-tBP的加标回收率平均值分别为88%~104%、83%~96%,相对标准偏差(RSD)分别为5.9%~8.2%、6.1%~13.0%。该方法成功应用于20份实际人血清中BPA和4-t-BP的分析,并且在血清中均检出BPA,但是未检出4-t-BP。结论该方法样品前处理简单快速,而且灵敏高,准确性好,适合于大规模人群血清中BPA和4-t-BP的分析。Objective To establish a method for the rapid determination of bisphenol A（ BPA） and 4- tert- butylphenol（ 4-t- BP） in human serum by ultra- performance liquid chromatography coupled to triple quadrupole mass spectrometry（ UPLC-Qq Q MS）. Methods After 200 μl of serum was hydrolyzed with β- glucuronidase,extracted by methyl- t- butyl ethyl,and derivatized with dansyl chloride,the derivatized products of BPA and 4- t- BP were separated on C18 UPLC column with the gradient elution of mobile phase of methanol and water containing 0. 1% formic acid,and quantified by Qq Q MS with internal standard calibration curve method. Results The linear correlation coefficients（ r） of BPA and 4- t- BP were greater than0. 995,and good linearity was obtained when the concentration of it was within 0. 1 ng / ml- 50 ng / ml; the limits of detection were 0. 05 ng / ml for BPA and 0. 07 ng / ml for 4- t- BP when the ratio of signal to noise was set to 3. The average recoveries of BPA and 4- t- BP,spiked at three different concentration levels of 1. 0 ng / ml,2. 0 ng / ml,and 10 ng / ml,were respectively within 88%- 104% and 83%- 96%,with the relative standard deviations（ RSDs） within 5. 9%- 8. 2% and 6. 1%- 13%.The method was successfully applied to the analysis of BPA and 4- t- BP in the serum of 20 patients,and BPA was detected in the serum,but the 4- t- BP was not detected. Conclusion The sample pretreatment of the method is simple and rapid,its sensitivity and accuracy are good. It is suitable for the determination of serum BPA and 4- t- BP in large scale human population survey.

关 键 词：血清 双酚A 4-叔丁基苯酚 超高效液相色谱串联质谱法 

分 类 号：O657.63[理学—分析化学]