超高效液相色谱-串联质谱法检测柴油中的微量蔗糖

目的建立检测柴油中微量蔗糖的超高效液相色谱-串联质谱(UPLC-MS/MS)方法。方法用纯水提取柴油样品中的蔗糖,以乙腈-水为流动相,梯度洗脱,经ZORBAX RX-SIL色谱柱(2.1mm×150mm,5μm)分离,以电喷雾离子源采用负离子扫描,多反应监测(MRM)进行数据分析。结果该方法检测下限(LOD)达10.0μg/L,定量限(LOQ)为15.0μg/L,在50.0~1000.0μg/L范围内线性关系良好;低、中、高3种浓度的加样回收率分别为85.5%、91.5%、90.3%,且相对标准偏差(RSD)均小于10%。结论该方法操作简单快速、灵敏度高、稳定性好、结果可靠,完全满足将蔗糖放入柴油中损坏机械设备案件检验的需求。

Determination of Trace Sucrose in Diesel Oil by UPLC-MS/MS

Objective To detect the trace sucrose in diesel oil by ultra-performance liquid chromatography in tandem with mass spectrum(UPLC-MS/MS).Methods Sucrose was extracted from the diesel oil sample through deionized water for analysis by UPLC-MS/MS,which was performed on a ZORBAX RX-SIL(2.1mm×150mm,5μm)column being fl owed with acetonitrile-water,the mobile phase,along with mass spectrometric acquisition being carried out by electrospray ionization in negative mode plus multiple reaction monitoring(MRM).Results The detected sucrose was of linear range among 50.0~1000.0μg/L,limits of detection(LOD)10.0μg/L and limits of quantifi cation(LOQ)15.0μg/L.The mean recoveries of low,middle and high concentrations were respective of 85.5%,91.5%,90.3%,bringing forth all of the relative standard deviation(RSD)less than 10%.Conclusions The method is simple,rapid,sensitive,stable and reliable,capable of being applied into forensic identifi cation.