固相萃取/高效液相色谱-串联质谱法测定人尿中8种有机磷酸酯阻燃剂代谢物  

Determination of Eight Metabolites of Organophosphate Flame Retardants in Human Urine by Solid-phase Extraction/High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：秦威振 黄承鹏 王甫 任燕 陆少游 罗兰 QIN Wei-zhen;HUANG Cheng-peng;WANG Fu;REN Yan;LU Shao-you;LUO Lan(Shenzhen Longhua District Center for Disease Control and Prevention,Shenzhen 518109,China;School of Public Health(Shenzhen),Sun Yat-sen University,Shenzhen 518107,China)

机构地区：[1]深圳市龙华区疾病预防控制中心,广东深圳518109 [2]中山大学公共卫生学院(深圳),广东深圳518107

出　　处：《分析测试学报》2025年第4期726-731,共6页Journal of Instrumental Analysis

基　　金：深圳市龙华区医疗卫生机构区级科研项目(2021100);深圳市科技计划项目(JCYJ2021032414181504)。

摘　　要：建立了检测人尿中8种有机磷酸酯阻燃剂代谢物(磷酸二苯酯、磷酸二甲苯酯、磷酸二邻甲苯酯&磷酸二对甲苯酯、磷酸二(1-氯-2-丙基)酯、磷酸二(1,3-二氯-2-丙基)酯、磷酸二(2-氯乙基)酯、磷酸二(2,3-二溴丙基)酯、磷酸二(2-丁氧基乙基)酯)的高效液相色谱-串联质谱法。取2 mL尿样,经酶解、净化、浓缩、复溶,采用1 mmol/L乙酸铵水溶液与甲醇为流动相梯度洗脱,Kinetex C_(18)(100 mm×2.1 mm,2.6μm)色谱柱分离,电离方式为电喷雾负离子模式,检测方式为多反应监测模式,内标法定量。在优化条件下,目标化合物在一定的质量浓度范围内呈良好线性关系,相关系数(r^(2))大于0.99,检出限为0.05~0.30μg/L,定量下限为0.20~1.0μg/L,平均回收率为76.8%~115%,相对标准偏差为2.3%~9.8%。该法简单快速、灵敏度高,已应用于深圳市龙华区儿童尿液中有机磷酸酯阻燃剂代谢物的含量分析,可为人群有机磷酸酯阻燃剂代谢物的暴露风险评估提供科学依据。A method was established for the determination of 8 diaryl phosphates(diphenyl phosphate,dibenzyl phosphate,bis(2-methylphenyl)hydrogen phosphate&bis(4-methylphenyl)hydrogen phosphate,bis(1-chloro-2-propyl)phosphate,bis(1,3-dichloro-2-propyl)phosphate,bis(2-chloroethyl)phosphate,bis(2,3-dibromopropyl)phosphate,bis(butoxyethyl)phosphate)in human urine using high performance liquid chromatography-tandem mass spectrometry.The target compounds were extracted,purified,concentrated and redissolved.Then,the target compounds were separated by a Kinetex C_(18)(100 mm×2.1 mm,2.6μm)column.1 mmol/L ammonium acetate aqueous solution and methanol were used as mobile phase and gradient elution was adopted.Quantitative analysis was performed using isotope internal standard under ESI-ion source mode.Under optimal conditions,the target compounds showed good linearity with the correlation coefficients(r^(2))greater than 0.99 within their respective ranges.The detection limits(LODs)were in the range of 0.05-0.30μg/L,and the quantification limits(LOQs)were in the range of 0.2-1.0μg/L.Average recoveries of the target compounds were in the range of 76.8%-115%at three different levels,and the relative standard deviations(RSDs)were between 2.3%and 9.8%.This method is simple,fast,highly sensitive and effective.It has been applied to analyze the levels of metabolites of organophosphate flame retardants in children’s urine in Longhua District,Shenzhen.It provides a scientific basis for the exposure assessment of metabolites of organophosphate flame retardants.

关 键 词：固相萃取 高效液相色谱-串联质谱 人尿 有机磷酸酯阻燃剂代谢物 

分 类 号：O657.7[理学—分析化学] X132[理学—化学]