摘要
建立了海洋生物体中16种优先控制多环芳烃的超声提取/气相色谱-质谱测定方法,对海洋鱼类、虾类、贝类和蟹类等生物样品的提取、净化和色谱质谱条件进行了优化。以正己烷-二氯甲烷(2∶1)作为溶剂进行超声提取,提取液经60%硫酸溶液和中性氧化铝-弗罗里硅土混合层析柱净化,采用气相色谱-质谱法定性和定量分析。在优化条件下,16种多环芳烃的线性范围为0.005～0.500 mg/L,相关系数(r)不低于0.998 4,检出限为0.03～0.28μg/kg。加标水平为2、20、100μg/kg时,平均加标回收率分别为55%～118%、80%～114%和79%～113%,相对标准偏差(RSDs,n=6)均小于10%。该方法快速、准确、灵敏度高、重复性好,能满足海洋生物体中持久性有机污染物分析的要求。
A GC -MS method was developed and validated for the determination of sixteen polycyclic aromatic hydrocarbons（PAHs） listed by the US Environmental Protection Agency as priority pollutants in marine organisms such as fish, shrimp, mussel, crab and the others. The procedures of extraction and purification, as well as chromatographic and mass spectrometric parameters, were optimized. The biological samples were extracted ultrasonically with hexane - dichloromethane （ 2 ： 1 ） mixture, and treated with 60% sulfuric acid, followed by clean-up with a glass column containing Florisil and neutral alumina. The analysis of target compounds was performed by gas chromatography - mass spectrometry （GC -MS）. Under the optimized conditions, the calibration curves of 16 PAHs were linear in the range of O. 005 -0. 500 mg./L with correlation coefficients（r） not less than 0. 998 4 and limits of de- tection of 0. 03 -0. 28 μg/kg. The average spiked recoveries for the fishery products at the spiked levels of 2, 20 and 100 μg/kg were in the range of 55% - 118% , 80% - 114% and 79% - 113% , respectively, with relative standard deviations （RSDs, n = 6 ） less than 10%. The results showed that the method is rapid, accurate, sensitive and reliable, and could satisfy the requirements for analysis on persistent organic pollutants （POPs） in marine organisms.
出处
《分析测试学报》
CAS
CSCD
北大核心
2013年第1期57-63,共7页
Journal of Instrumental Analysis
基金
国家科技支撑计划重大课题(2009BADB7B02)
中央级公益性科研院所基本科研业务费专项(中国水产科学研究院南海水产研究所)资助项目(2012TS15)
关键词
超声提取
气相色谱-质谱
多环芳烃
海洋生物体
ultrasonic extraction
gas chromatography -mass spectrometry
polycyclic aromatic hy-drocarbons
marine organisms
