液相色谱-电喷雾串联质谱法测定饮用水中的萘二酚类物质

建立了饮用水中七种萘二酚的液相色谱-电喷雾串联质谱分析方法。样品用C18固相萃取柱富集,经滤膜过滤后进样,以甲醇-水为流动相,梯度洗脱,经C18柱分离后,采用多反应监测(MRM)负离子模式检测,外标法定量。空白样品及其添加实验结果表明,特征离子相对强度的比值稳定,无基质干扰,结合保留时间可实现准确的定性定量。在优化实验条件下,萘二酚类物质线性范围为0.50~50μg/L,线性关系良好,相关系数均大于0.998。方法检出限(以信噪比为3计)为1.0~3.0 ng/L,方法定量限(以信噪比为10计)为4.0~10 ng/L,井水、自来水、矿泉水样品添加水平为4.0~50 ng/L时,回收率为81.4%~112%,相对标准偏差(n=6)为2.1%~7.8%。该方法有前处理简单、回收率高、精密度好,灵敏度高,选择性强的优点,适用于饮用水中萘二酚类物质的测定。

Simultaneous Determination of Naphthalenediols in Drinking Water by SPE-HPLC-MS/MS

A new method for the determination of seven naphthalenediols in water by liquid chromatography-electrospray ionization tandem mass spectrometry(HPLC-MS/MS) was established.The sample was extracted with a C18 cartridge,and then separated by HPLC-MS/MS using a C18 column with methanol aqueous solution as the mobile phase for gradient elution.And the tandem mass spectral acquisition was done in the negative electrospray ionization utilizing multiple reaction monitoring.External standard method was applied for quantization.The result indicated that the limits of determination(LODs) of seven naphthalenediols were ranged from 1.0 ng/L to 3.0 ng/ L(S/N=3),limits of quantification(LOQs) were ranged from 4.0 ng/L to 10 ng/ L(S/N=10);meanwhile,the linear correlation coefficients of seven naphthalenediols were all greater than 0.998 within the irrespective linear ranges.The mean recoveries for well water,tap water and mineral water samples at three spiked concentrations levels of 4.0-50 ng/L were ranged from 81.4% to 112% with RSD of 2.1%-7.8%(n=6).Analysis of blank and fortified samples showed that the relative intensity of the seven naphthalenediols were stable.And there was no matrix interference with these diagnostic ion pairs.Combining with retention time,the method could be used for accurate qualitative analysis.