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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 for the determination of nicotine in e-liquid by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS / MS) was established. Samples were extracted by acetonitrile solution and determined by ultrasonic extraction. Separation was performed on a Waters Atlantis T3 (3 μm, 2.1 × 100 mm) column using a gradient elution with acetonitrile-water as the mobile phase at a column temperature of 35 ° C at a flow rate of 0.3 mL / min and electrospray positive ion mode Data, external standard method. The experimental results showed that the linear range of nicotine was 0.01-5 mg / L, R2 was 0.9999, the spiked recoveries were 99.2%, the limits of detection and the limits of determination were 0.001 mg / L and 0.01 mg / L, respectively , RSD was 0.23%. In the actual sample test, there was a big difference between the identification amount and the detection volume of the e-liquid; the smoke liquid marked as high-school concentration showed a negative difference, and the smoke liquid labeled as low concentration and zero concentration showed a positive difference; The size of the difference between the size of the logo and taste of liquid smoke has nothing to do.