摘要
建立了一种测定烟用接装纸中18种邻苯二甲酸酯类(PAEs)化合物的液相色谱-串联质谱(LC-MS/MS)法。剪碎后的样品用水浸润,加入乙醇超声萃取,提取液过0.22μm有机相滤膜后进行LC—MS/MS分析。结果表明:①以甲醇-5mmol/L乙酸铵的乙酸水溶液(乙酸和水体积比1:1000)为流动相,流速0.4mL/min进行梯度洗脱,18种PAEs在9min内得到良好分离,采用多反应监测(MRM)模式进行定性和定量分析,方法快速可靠,线性范围为1~500ng/mL,定性检出限为0.01~1.85mg/kg(S/N=3)。②该方法用于检测烟用接装纸中18种PAEs,操作简单快捷,回收率在82.8%~111.6%之间,相对标准偏差(RSD)小于10%。
A method for determining 18 phthalate compounds in tipping paper was developed with liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were ultrasonically extracted with ethanol after soaking with water. Then the extract was analyzed with LC-MS/MS after passing through of an organic phase membrane filter of 0.22μm. The results showed that : l) The targeted phthalate compounds could be well separated in 9 minutes with gradient elution by using methanol and 5 mmol/L ammonium acetate in acetic acid-water solution (1 : 1000, V/V) as the mobile phase at a flow rate of 0.4 mL/min. Multiple reaction monitoring (MRM) mode was adopted for qualitative and quantitative analyses. This method was reliable with the linear range of 1-500 ng/mL and the qualitative detection limit of 0.01-1.85 mg/kg (S/N=3). 2) With the recovery of 82.8%-111.6% and the relative standard deviation (RSD) of less than 10%, this method featured good reproducibility.
出处
《烟草科技》
EI
CAS
北大核心
2013年第12期31-35,共5页
Tobacco Science & Technology