烟草科技2017，Vol.50Issue(2)：48-56,9.
在线二维固相萃取-HPLC-MS/MS法测定卷烟侧流烟气中的TSNAs
Determination of TSNAs in sidestream cigarette smoke by online two-dimensional solid phase extraction combined with HPLC-MS/MS
摘要
Abstract
In order to quantify four tobacco-specific N-nitrosamines (TSNAs) in sidestream cigarette smoke accurately, an online two-dimensional solid-phase extraction-liquid chromatography-tandem mass spectrometry (Online 2D SPE-HPLC-MS/MS) method was developed. Sidestream cigarette smoke was collected in a pre-treated (with ascorbic acid) fishtail chimney and a pre-treated (with ascorbic acid) Cambridge filter pad. The Cambridge filter pad post smoking was placed in an Erlenmeyer flask, and TSNAs adsorbed on fishtail chimney was rinsed by ammonium acetate solution. After extraction, the solution was filtered and cleaned by online 2D SPE, and analyzed by LC-MS/MS. The results showed that: 1) Comparing with online SPE on a single cation exchange cartridge or a single reversed phase cartridge, 2D SPE gave the best overall cleanup, removed interfering substances more effectively, and minimized any sample matrix effect. 2) The optimized 2D SPE conditions were: sample loading 0.8 mL of 2% FA at a flow rate of 1.0 mL/min, sample transferring 0.8 mL of 1% NH4OH at a flow rate of 0.8 mL/min, washing liquid for PRS cartridge 2% FA containing 15%MeOH, washing liquid for C18 HD cartridge 1% NH4OH, and elution time 1.5 min. 3) The detection limits forNNN, NAB, NAT and NNK were 0.006, 0.002, 0.004 and 0.003 ng/mL, respectively. The recoveries ranged from 93.4% to 107.3% and the relative standard deviations were less than 8%.This new approach is sensitive, accurate and suitable for the determination of NNN, NAB, NAT and NNK in sidestream cigarette smoke.关键词
在线二维固相萃取/高效液相色谱-串联质谱/烟草特有N-亚硝胺/卷烟/侧流烟气Key words
Online two-dimensional solid-phase extraction/HPLC-MS/MS/Tobacco-specific N-nitrosamine (TSNA)/Cigarette/Sidestream cigarette smoke分类
轻工纺织引用本文复制引用
张杰,白若石,杨振东,易小丽,周骏..在线二维固相萃取-HPLC-MS/MS法测定卷烟侧流烟气中的TSNAs[J].烟草科技,2017,50(2):48-56,9.基金项目
国家烟草专卖局科技重大专项项目"降低国产白肋烟、马里兰烟TSNAs含量关键技术研究"[110201301022 (JH-03)]. （JH-03）
