Fisheries College of Zhejiang Ocean University, Zhoushan, P. R. China.
Key Laboratory of Sustainable Utilization of Technology Research for Fishery Resource of Zhejiang Province, Marine Fishery Institute of Zhejiang Province, Zhoushan, P. R. China.
J Sep Sci. 2018 May;41(10):2188-2196. doi: 10.1002/jssc.201701229. Epub 2018 Apr 3.
We propose a method for the simultaneous determination of 15 kinds of polycyclic aromatic hydrocarbons in marine samples (muscle) employing gas chromatography with mass spectrometry after saponification with ultrasound-assisted extraction and solid-phase extraction. The experimental conditions were optimized by the response surface method. In addition, the effects of different lyes and extractants on polycyclic aromatic hydrocarbons extraction were discussed, and saturated sodium carbonate was first used as the primary saponification reaction and extracted with 10 mL of ethyl acetate and secondly 1 mol/L of sodium hydroxide and 10 mL of n-hexane were used to achieve better results. The average recovery was 67-112%. Satisfactory data showed that the method has good reproducibility with a relative standard deviation of <13%. The detection limits of polycyclic aromatic hydrocarbons were 0.02-0.13 ng/g. Compared with other methods, this method has the advantages of simple pretreatment, low solvent consumption, maximum polycyclic aromatic hydrocarbons extraction, the fast separation speed, and the high extraction efficiency. It is concluded that this method meets the batch processing requirements of the sample and can also be used to determine polycyclic aromatic hydrocarbons in other high-fat (fish, shrimp, crab, shellfish) biological samples.
我们提出了一种采用超声辅助提取和固相萃取后用气相色谱质谱法同时测定海洋样品（肌肉）中 15 种多环芳烃的方法。通过响应面法优化了实验条件。此外，还讨论了不同的碱和萃取剂对多环芳烃提取的影响，首次使用饱和碳酸钠作为主要的皂化反应，并用 10 mL 乙酸乙酯和其次 1 mol/L 氢氧化钠和 10 mL 正己烷进行萃取，以获得更好的结果。平均回收率为 67-112%。令人满意的数据表明，该方法具有良好的重现性，相对标准偏差小于 13%。多环芳烃的检测限为 0.02-0.13 ng/g。与其他方法相比，该方法预处理简单，溶剂消耗低，多环芳烃提取量最大，分离速度快，提取效率高。结论是，该方法满足样品的批量处理要求，也可用于测定其他高脂肪（鱼、虾、蟹、贝类）生物样品中的多环芳烃。
