液相色谱/串联质谱法测定水中邻苯二甲酸酯类化合物

Determination of six phthalate acid ester residues in water by ultra performance liquid chromatographytandem mass spectrometry

建立了直接进样-超高效液相色谱/三重四极杆串联质谱法同时测定水中6种邻苯二甲酸酯类化合物的方法。水样经离心后取上清液进样,采用BEH C18柱,以水(0.1%甲酸)-乙腈作为流动相进行梯度洗脱,采用串联质谱进行检测。实验通过在液相色谱系统中装入一根吸附分配柱,很好地解决了液相色谱系统的干扰问题。6种邻苯二甲酸酯类在一定范围内线性良好(r=0.9990~0.9996),回收率为84.3%~102%,相对标准偏差为1.0%~8.7%,方法检出限为0.05~0.5μg/L。方法适用于测定地表水中6种邻苯二甲酸酯类化合物的残留。

A method for analysis of six phthalate acid ester residues in water was developed performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. The water samples directly after centrifugation. A BEH C^s column was used for the liquid chromatographic separation, gradient elution program of acetonitrile -0. 1% formic acid as the mobile spectrometer equipped with an electrospray ionization source was phase. operated in the using ultra- were injected with a linear A triple quadrupole mass negative ion with multiple reaction monitoring mode （MRM）. By installing a chromatographic column, the interference problem of liquid chromatographic system was solved well. During the concentration range of 2.0 - 100μg/L, there was good linear relationship （r = 0. 9990 - 0. 9996 ） for all the six phthalate acid esters. The recoveries ranged from 84. 3% to 102%, with the relative standard deviations of 1.0% - 8.7%. The detection limits were between 0. 05 and 0. 5 μg/L. The method was suitable for the simultaneous determination of six phthalate acid esters in surface water.