摘要
建立超高效液相色谱-串联质谱法测定血清中双酚A、双酚F、双酚S 3种双酚类化合物和4-壬基酚。血清样本经甲醇提取、沉淀蛋白质,提取液用ACQUITY UPLC BEH C18色谱柱分离,以0.01%(体积分数)氨水溶液和甲醇为流动相进行梯度洗脱,在电喷雾负离子模式下,采用多反应监测模式检测,用同位素内标法定量。4种目标化合物的质量浓度在0.1~20μg/L范围内与色谱峰面积线性关系良好,相关系数均不小于0.995,方法检出限为0.03~0.1μg/L,定量限为0.1~0.3μg/L。样品加标平均回收率为83.6%~93.2%,测定结果的相对标准偏差为4.8%~7.8%(n=6)。该方法适用于人体血清中双酚A、双酚F、双酚S 3种双酚类化合物和4-壬基酚的测定。
A method of ultra-performance liquid chromatography-tandem mass spectrometry was established for the determination of bisphenol A,bisphenol F,bisphenol S and 4-nonylphenol in serum.Serum samples were extracted with methanol to precipitate proteins.The extract was separated with ACQUITY UPLC BEH C18 chromatographic column.The gradient elution was carried out with 0.01%(volume fraction)ammonia solution and methanol as mobile phase.Detection was performed under the electric spray negative ion mode using multiple reaction monitoring(MRM),and quantification was carried out using the isotope-labeled internal standard method.The mass concentration of the four target compounds had good linear relationship with the chromatographic peak area in the range of 0.1-20μg/L,with correlation coefficients not less than 0.995.The detection limits of the method were 0.03-0.1μg/L,and the quantification limits were 0.1-0.3μg/L.The average recoveries of samples spiked were 83.6%-93.2%,and the relative standard deviations of the determination results of six parallel samples were 4.8%-7.8%.This method is suitable for the determination of bisphenol A,bisphenol F,bisphenol S and 4-nonylphenol in human serum.
作者
崔泓
陈红霞
杜云
CUI Hong;CHEN Hongxia;DU Yun(Testing and Inspection Center of Shiyan Centers for Disease Control and Prevention,Shiyan Health Supervision Institute,Shiyan 442000,China;Institute of Biomedicine,Taihe Hospital,Hubei University of Medicine,Shiyan 442000,China)
出处
《化学分析计量》
2026年第1期100-104,154,共6页
Chemical Analysis And Meterage
基金
2025年湖北省肝癌精准诊疗临床医学研究中心开放课题(2025LCOF10)。
关键词
双酚类化合物
壬基酚
血清
超高效液相色谱-串联质谱法
bisphenol compounds
nonylphenol
serum
ultra-performance liquid chromatography-tandem mass spectrometry
