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.pdfVIP

Modern Food Science and Technology 2012, Vol.28, No.5 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 黄金凤，林森煜，何敏恒，李秀英，郭新东，吴玉銮 (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) 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 ~ 50 µg/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。 关键词：萘二酚；饮用水；固相萃取；液相色谱-电喷雾串联质谱 文章篇号：1673-9078(2012)5-583-587 Simultaneous Determination of Naphthalenediols in Drinking Water by SPE-HPLC-MS/MS HUANG Jin-feng, LIN Sen-yu, HE Min-heng, LI Xiu-ying, GUO Xin-dong, WU Yu-luan (Guangzhou Quality Supervision and Testing Institute, National Centre for Quality Supervision and Testing of Processed Food (Guangzhou), Guangzhou City Key Laboratory of Detection Technology for Food Safety, Guangzhou City Research Center of Risk Dynamic Detection and Early Warning for Food Safety,Guangzhou Guangdong 510110, China) Abstract: 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 C column with methanol aqueous solution as the mobile phase for gradient elution. And the tandem mass spectral 18 acquisition was done in the negative electrospray ionization utilizing multiple rea