气相色谱-串联质谱法测定船用燃料油中的9种含氮化合物

采用气相色谱-串联质谱(GC-MS/MS)法建立了船用燃料油中9种含氮化合物的测定方法。样品以SPE小柱净化去除饱和烃后,通过二氯甲烷-乙醇(5∶1)溶液洗脱。用DB-5MS(30 m×0.25 mm×0.25μm)色谱柱分离,采用多反应监测(MRM)模式,外标法定量。结果表明,9种含氮化合物的色谱分离效果良好,在浓度1~1 000 mg/kg范围内与峰面积均呈线性关系。方法的定量下限(S/N=10)为0.18~0.43 mg/kg,平均加标回收率为85.3%~121.6%,相对标准偏差(RSD,n=6)均不大于6.8%。结果表明该方法快速可靠、准确简便,适用于船用燃料油中9种含氮化合物的检测。

Determination of 9 Nitrogen-containing Compounds in Marine Fuel Oil by Gas Chromatography-Tandem Mass Spectrometry

A gas chromatography-tandem mass spectrometric method was developed for the determination of 9 nitrogen-containing compounds in marine fuel oil.The sample was purified with SPE cartridge to remove the saturated hydrocarbon,and then eluted with a mixed solution composing of dichloromethane and ethanol(5 ∶ 1).The target ingredients were separated on a DB-SMS column(30 m ×0.25 mm ×0.25 μm),detected in multiple-reaction monitoring mode(MRM),and quantified by the external standard method.The method indicated a perfect performance in chromatographic separation.The linear ranges of 9 nitrogen-containing compounds were between 1 mg/kg and 1 000 mg/kg,and the limits of quantitation were between 0.18 mg/kg and 0.43 mg/kg.The recoveries ranged from 85.3％ to 121.6％,with relative standard deviations(RSDs,n =6) less than 6.8％.This method was rapid,accurate,precise and convenient to operate,and it was appropriate for the determination of 9 nitrogen-containing compounds in marine fuel oil.