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  

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

作　　者：黄金凤 林森煜 何敏恒 李秀英 郭新东 吴玉銮 

机构地区：[1]广州市质量监督检测研究院,国家加工食品质量监督检验中心(广州),广州市食品安全检测技术重点实验室,广州市食品安全风险动态监测与预警研究中心,广东广州510110

出　　处：《现代食品科技》2012年第5期583-587,共5页Modern Food Science and Technology

基　　金：广州市科技计划项目(广州市食品安全检测技术重点实验室[2011]233-34)

摘　　要：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1.0-3.0ng／L，方法定量限（以信噪比为10计）为4．0-10ng／L，井水、自来水、矿泉水样品添加水平为4.0-50ng／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l生强的优点，适用于饮用水中萘二酚类物质的测定。A new method for the detenuination of seven naphthalenediols in water by liquid chromatography-electrospray ionization tandem mass spectrometry （HPLC-MS/MS） was established. The sample was extracted with a Cl8 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 eleclrospray 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.

关 键 词：萘二酚 饮用水 固相萃取 液相色谱-电喷雾串联质谱 

分 类 号：R123.1[医药卫生—环境卫生学] O657.63[医药卫生—公共卫生与预防医学]