人体血清中6种邻苯二甲酸酯的气相色谱-质谱同时测定法

目的 建立一种同时测定人体血清中6种邻苯二甲酸酯(PAEs)的方法,并在此基础上了解人体内PAEs污染水平.方法 运用超声萃取,以气相色谱-质谱-选择离子检测(GC-MS-SIM)和内标法定量等方法对人体血清中6种PAEs进行同时测定,并运用于50份实际血清样品的检测.结果 该方法在10～1000 ng/ml范围内线性关系良好,标准曲线回归方程拟合度R~2均＞0.999;空白加标中平均回收率为94.5%,相对标准偏差(RSD,n=6)为4.4%;邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸(2-乙基己基)酯(DEHP)、邻苯二甲酸二辛酯(DNOP)的最低检出限分别为0.31、0.85、0.90、0.63、0.88和0.41 ng/ml,所有实际样品加标回收率为67.98%～110.8%.结论 该方法回收率和重现性良好,检测限较低,可用于人体血清中多种PAEs类物质的同时检测.

Abstract：

Objective To establish a method to determine six kinds of PAEs in human serum simultaneously,and on this basis to understand the level of PAEs in human body.Methods Uhrasonic extraction,gas chromatography-mass spectrometryselected ion monitoring (GC-MS-SIM) detection and quantitative analysis based on internal standard were used to detect six kinds of PAEs in human serum simultaneously.Finally this method was used in fifty human serum samples.Results The results showed that this method had a good linear relation in the range from 10 to 1 000 ng/ml.and the correlation coefficients of standard curve were higher than 0.999.The average recovery rate and the relative standard deviation(RSD,n=6)of the target compounds in standard-addition blank was 94.5%and 4.4%respectively,the lower limits of detection for DEP,DMP,DBP,BBP,DEHP,DNOP were0.31,0.85,0.90,0.63,0.88,0.41 ng/ml respectively,and the recovery rates of all samples ranged from 67.98%to 110.8%.Conclusion This method has good recovery rate,reproducibility,lower limit of detection and can be used for the determination of many kinds of PAEs substances in human serum.

Simultaneous Determination of Six Kinds of Phthalic Acid Esters in Human Serum by Gas Chromatography-Mass

Objective To establish a method to determine six kinds of PAEs in human serum simultaneously,and on this basis to understand the level of PAEs in human body.Methods Uhrasonic extraction,gas chromatography-mass spectrometryselected ion monitoring (GC-MS-SIM) detection and quantitative analysis based on internal standard were used to detect six kinds of PAEs in human serum simultaneously.Finally this method was used in fifty human serum samples.Results The results showed that this method had a good linear relation in the range from 10 to 1 000 ng/ml.and the correlation coefficients of standard curve were higher than 0.999.The average recovery rate and the relative standard deviation(RSD,n=6)of the target compounds in standard-addition blank was 94.5%and 4.4%respectively,the lower limits of detection for DEP,DMP,DBP,BBP,DEHP,DNOP were0.31,0.85,0.90,0.63,0.88,0.41 ng/ml respectively,and the recovery rates of all samples ranged from 67.98%to 110.8%.Conclusion This method has good recovery rate,reproducibility,lower limit of detection and can be used for the determination of many kinds of PAEs substances in human serum.