| 摘要: |
| 海洋生物体中的石油烃质量分数是海洋环境监测评价体系的重要指标，现行分析方法标准为《海洋监测规范 第6部分：生物体分析》（GB 17378.6—2007）荧光分光光度法，该标准方法中前处理操作较为复杂，实际样品分析中存在样品平行性差、加标回收率范围宽等问题。由于样品均匀性、皂化进程、萃取分离操作手法等因素均会影响样品测定结果的平行性和精密度水平。因此，对比了不同制备方式的样品（干样和匀浆样），通过过滤或离心的方式去除了皂化液中的非石油烃大分子干扰；并对比了不同皂化温度和时间，获得了最优的前处理方法，提升了方法的准确度和精密度。对实际海洋生物体样品的分析表明，优化后的方法检出限为0.9 mg/kg，变异系数为7.02%~14.4%，加标回收率为67.4%~138%，精密度和准确度良好，基本满足海洋生物体中石油烃测定的要求。 |
| 关键词: 海洋生物体 石油烃 荧光分光光度法 大分子干扰 过滤 离心 |
| DOI： |
| 分类号:X834 |
| 基金项目:江苏省环境监测科研基金资助项目（2103，2002） |
|
| Optimization of Pre treatment Methods for Fluorescence Spectrophotometric Analysis of Petroleum Hydrocarbons in Marine Organisms |
|
FU Dan，YAN Li，YUAN Guangwang，LV Ying，SUN Qi，WANG Hui1,2
|
|
1.Jiangsu Provincial Environmental Monitoring Center， Nanjing，Jiangsu 210019，China;2. Jiangsu Marine Environmental Monitoring Forecasting Center， Nanjing，Jiangsu 210019，China
|
| Abstract: |
| Petroleum hydrocarbon in marine organisms is an important indicator of the marine environmental monitoring and evaluation mechanism. It is analyzed by fluorescence spectrophotometric method using “Marine Monitoring Specification Part 6： Analysis of Organisms” (GB 17378.6—2007). However， due to the complexity of the pre treatment operation in the standard method， problems such as poor parallelism and wide range of spiked recoveries were found in the actual sample analysis. As sample homogeneity， saponification process and extraction practices can affect detection parallelism and precision， different sample preparation methods (dry and homogenised samples) were contrasted and filtration or centrifugation was used to remove non petroleum hydrocarbon macromolecule interference from the saponification solution. In addition， different saponification temperature and time were compared to obtain appropriate pre treatment operation. The accuracy and precision of the method were improved by comprehensive improvements to the current standard. The analysis of marine organism samples showed that the detection limit of the method was 0.9 mg/kg， the precision level was 7.02%~14.4%， and the spiked recovery ranged from 67.4% to 138% with well reproducibility. This study provides a technical basis for the marine environmental monitoring and evaluation system. |
| Key words: Marine organisms Petroleum hydrocarbons Fluorescence spectrophotometry Macromolecular interference Filtration Centrifugation |
