固相萃取-超高效液相色谱/三重四极杆质谱法同时测定地表水中8种亚硝胺类化合物

Simultaneous Determination of Eight Nitrosamines in Surface Water by Solid Phase Extraction and Ultra-performance Liquid Chromatography Tandem Triple Quadrupole Mass Spectrometry

建立了固相萃取(SPE)-超高效液相色谱/三重四极杆串联质谱(UPLC-MS/MS)同时测定地表水中8种亚硝胺类化合物的方法。水样中目标物经椰壳活性炭固相萃取小柱吸附富集,小柱经氮气吹干后采用二氯甲烷洗脱。待测样品采用Atlantis T3柱,以水-甲醇作为流动相进行梯度洗脱,大气压力化学电离源(APCI)正离子模式多反应监测方式(MRM)进行检测,内标法定量分析。8种目标物在相关线性范围内线性良好(r≥0.9950),地表水加标回收率为55.4%~90.4%,相对标准偏差为3.1%~14.3%,方法检出限为1.1~1.8 ng/L。本方法准确度和灵敏度高,适用于快速测定地表水中8种亚硝胺类化合物含量。

A method for analysis of eight nitrosamines in surface water was developed using solid phase extraction(SPE)and ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were extracted and cleaned with coconut charcoal solid phase extraction cartridges.After drying by nitrogen,the cartridges were eluted with dichloromethane.The Atlantis T3 column was used for the liquid chromatography separation,with a linear gradient elution program of methanol-water as the mobile phase.A triple quadrupole mass spectrometer equipped with an atmospheric-pressure chemical ionization was operated in the positive ion with multiple reaction monitoring mode(MRM),and internal standard method was used for quantitation.There were good linear relations(r≥0.9950)of all the 8 nitrosamines.The recoveries ranged from 55.4%to 90.4%,with the relative standard deviations of 3.1%~14.3%.The detection limits were between 1.1~1.8 ng/L.The method is sensitive and accurate,and is suitable for simultaneous determination of eight nitrosamines residues in surface water.