Shao Bing, Hu Jian-Ying, Yang Min
State Key Laboratory of Environmental Aquatic Chemistry, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing.
J Chromatogr A. 2002 Mar 15;950(1-2):167-74. doi: 10.1016/s0021-9673(02)00011-0.
A comprehensive analytical method based on normal-phase liquid chromatography-electrospray ionization mass spectrometry (NPLC-ESI-MS) has been established for determination of nonylphenol ethoxylates (NPEOs) in the aquatic environment. Extraction and cleanup of samples were performed on graphitized carbon black (GCB) solid-phase extraction cartridges. Complete separation between each individual NPEOs was achieved by combining a C18 pre-column with a silica analytical column and using acetonitrile-water as eluent. Quantitative determination by LC-ESI-MS was achieved in the positive ionization (PI) mode at a ramped cone voltage for NPEOs using selected ion monitoring. Recoveries for NPEOs ranged between 91.9 and 117.5%, and the limits of detection varied between 0.5 and 2 ng/l for individual NPEOs with n longer than 2, and between 5 and 0.5 microg/l for NPIEO and NP2EO. This method was successfully applied to the investigation of residual NPEOs with n>2 in the Chongqing area of the Changjiang river. NPEOs with n ranging from 1 to 22 were found to vary between 0.1 and 2900 ng/l with a distribution depending on the depth of water.
建立了一种基于正相液相色谱 - 电喷雾电离质谱法(NPLC - ESI - MS)的综合分析方法,用于测定水环境中的壬基酚聚氧乙烯醚(NPEOs)。样品的萃取和净化在石墨化炭黑(GCB)固相萃取柱上进行。通过将C18预柱与硅胶分析柱联用,并以乙腈 - 水作为洗脱剂,实现了各NPEOs之间的完全分离。使用选择离子监测,在正离子(PI)模式下,通过对NPEOs采用梯度锥电压,实现了LC - ESI - MS的定量测定。NPEOs的回收率在91.9%至117.5%之间,对于n大于2的单个NPEOs,检测限在0.5至2 ng/L之间,对于NPIEO和NP2EO,检测限在5至0.5 μg/L之间。该方法成功应用于长江重庆段n>2的残留NPEOs的调查。发现n为1至22的NPEOs含量在0.1至2900 ng/L之间,其分布取决于水的深度。