超高效液相色谱-三重四极杆质谱测定沉积物中6种对羟基苯甲酸酯及其代谢产物

Determination of Paraben and Its Metabolite in Sediments by Ultra Performance Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry

建立了一种测定沉积物中6种对羟基苯甲酸酯类化合物及其代谢产物对羟基苯甲酸的定量分析方法。样品用甲醇-水(5∶3,V/V)混合液进行两次提取,经Oasis MCX固相萃取柱净化,采用UPLC~HSS T3色谱柱分离,以甲醇-0.1%(V/V)甲酸溶液为流动相进行梯度洗脱,在多反应监测(MRM)模式下进行定性分析,内标法进行定量分析。结果表明,7种目标物质在0.1~500.0μg/L范围内有良好的线性关系(r≥0.9995),方法定量限为0.75~1.23 ng/g,回收率为65.5%~88.3%,相对标准偏差为7.4%~13.6%。本方法前处理简单,灵敏度高,选择性好,可用于沉积物中对羟基苯甲酸酯类化合物的测定。

A new method for simultaneous determination of six benzoic acid esters and their metabolite phydroxybenzoic acid( p-HB) in sediments was developed. The samples were extracted with methanol and water,and then the extraction was purified by Oasis MCX solid phase column. The separation of targets was conducted by passing through a UPLC~HSS T3 column with a methanol-0. 1% acid aqueous solution as the mobile phase under gradient elution. The qualitative analysis of the analytes was measured by Ultra performance liquid chromatography-Triple quadrupole tandem mass under multiple reaction monitoring mode( MRM) and the internal standard method was applied for quantitative analysis. The results indicated that seven target substances had a good linear relationship in the range of 0. 1-500 μg/L with correlation coefficients above 0.9995 and the detection limits of 0.75-1.23 ng/g. The recoveries ranged from 65.5% to 88.3% and the relative standard deviation was 7. 4%-13. 6%. This method was suitable for the measurement of benzoic acid esters with the advantages such as simple processing,good selectivity and high sensitivity.