超高效液相色谱-串联质谱法测定电子烟液中烟碱

Determination of nicotine by UPLC-MS/MS in electronic cigarette liquid

建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)测定电子烟液中烟碱的方法。样品经乙腈溶液提取,超声萃取后测定。以乙腈-水作为流动相进行梯度洗脱,在Waters Atlantis T3(3μm,2.1×100 mm)色谱柱上进行分离,柱温35℃,流速0.3 m L/min,在电喷雾正离子模式下采集数据,外标法定量。实验结果表明:烟碱质量浓度在0.01~5 mg/L范围内线性良好,R2为0.9999,加标回收率为99.2%,检出限及测定低限分别为0.001 mg/L及0.01 mg/L,RSD为0.23%。实际样品检测中电子烟液标识量和检测量差异大;标识为高中浓度的烟液表现为负差异,标识为低浓度及零浓度的烟液表现为正差异;烟碱的标识量和实测量的差异大小与烟液的标识口味无关。

A method was established for nicotine detection in electronic cigarette liquid by UPLC-MS/MS.The analytes were extracted from the sample by acetonitrile with the assistance of ultrasound.The sample was analysed in electrospray positive ion and multiple reaction mode after separation on a Waters Atlantis T3（3 μm 2.1 × 100 mm） column with acetonitrile or water as mobile phase.The flow rate was adjusted to 0.3 mL/min,and the column temperature was set as 35℃.The analytes were quantified by external standard method.The results indicated that this method exhibited a good linearity with R^2= 0.9999 in the range of 0.01 - 5 mg/L.The average recovery was 99.2 %,and the LODs and LOQs of this method were 0.001 mg/L and 0.01 mg/L,with the RSD of 0.23 %.There was a large difference between the labeled quantity and actual detection.The labeled highmedium concentration presented negative difference,while the labeled low concentration and zero concentration presented positive difference.Furthermore,the cigarette taste is irrelevant to how much the detected value differed from the labeled quality.