本文利用乙酸银修饰的氧化铝-硅胶材料制备固相萃取柱对船用残渣燃料油样品进行净化分离,结合气相色谱-串联质谱技术,使用DB-35 MS UI色谱柱分离,多反应监控模式,内标法定量测定酚类及脂肪酸甲酯(FAME)类化合物.对影响酚类和FAME类化合物的进样方式、萃取溶剂的选择、固相萃取柱类型的选择以及淋洗和洗脱条件进行了优化,建立了船用残渣燃料油中酚类及FAME类化合物的测定方法.方法在浓度0.05～2.5 μg/mL范围线性良好,具有检出限(0.1～1.2 mg/kg)和定量限(0.3～4.0 mg/kg)低,稳定性好和萃取效率高,以及基质效应不显著等优势.通过用不含目标物的空白燃料油配制0.10、0.50、2.50 mg/L浓度水平的试样考察方法的可靠性,获得满意的回收率(85.5％～115.4％)和相对标准偏差(RSD≤6.2％).实验结果表明,建立的方法可实现船用残渣燃料油中酚类及FAME类化合物的有效检测.另外,劣质船用燃油存在不少的酚类和FAME类物质,高浓度苯酚、甲酚、二甲酚、对枯基苯酚、脂肪酸甲酯等物质可能是导致船舶油泵损坏的重要原因.
Determination of Phenols and Fatty Acid Methyl Esters Compounds in Bunker Residual Fuel Oil by Solid Phose Extraction-Gas Chromatography Triple Quadrupole Mass Spectrometry
In this paper,phenols and fatty acid methyl esters(FAMZ)in the marine residual fuel oil samples were purified and separated by a solid phase extraction column prepared with silver acetate modified alumina-silica gel material.Followed by gas chromatography-triple quadrupole mass spectrometry,DB-35 MS UI column was used for separation,multiple reaction monitoring mode,and internal standard method was used for quantification.We optimized the injection mode,extraction solvents,SPE columns,leaching and elution conditions which affected the response of phenols and FAME compounds.The method has the advantages of good linearity,the curves of the compounds were linear in the concentration range from 0.05 to 2.50 μg/mL,the limit of detection was 0.1-1.2 mg/kg,and the limit of quantitation was 0.3-4.0 mg/kg,The method has good stability and extraction efficiency,Matrix effect are not significant.Three spikes(0.10,0.50 and 2.50 mg/L)of blank residual fuel oil sample without target compounds were prepared to test the reliability of the method.Satisfactory recoveries(85.5％-115.4％)and relative standard deviations(RSD≤6.2％)were obtained.The experimental results show that the established method can effectively detect phenols and FAME compounds in marine residual fuel oil.In addition,there are many phenols and FAME substances in inferior fuel oil,such as phenol,methylphenol,ethylphenol,dimethylphenol,p-cumyl phenol,methyl hexadecarbonate and methyl octaenoate were detected.High concentration of phenols and FAME compounds may be one of the important reasons for the damage of ship oil pumps,which requires our high attention.
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