），俗名烟碱，是一种存在于茄科植物（茄属）中的生物碱，也是烟草的重要成分之一。 Nicotine , commonly known as nicotine, is an alkaloid found in the Solanaceae (Solanum) and one of the important components of tobacco. Nicotine can be addictive or dependent. Repeated use can lead to increased heart speed, increased blood pressure, and decreased appetite. Ingestion of large doses of nicotine can cause nausea and even vomiting, which can seriously cause death. ），采用气相色谱分离和电子轰击电离源（ EI ）配合全扫描模式完成定性分析， GCMS-SIM模式实现定量分析，可应用于烟草中尼古丁的检测。 Gas chromatography-mass spectrometer ( GCMS ), using gas chromatography separation and electron impact ionization source ( EI ) to complete the qualitative analysis in full scan mode, GCMS-SIM mode to achieve quantitative analysis, can be applied to the detection of nicotine in tobacco.
1.Introduction to the instrument
GC-MS 6800 is a cost-effective gas chromatograph / mass spectrometer carefully built by Skyray Instrument. , Petrochemicals, food safety, textile and leather and other industries in the detection of harmful substances.
气相色谱质谱联用仪外观图 Figure 1. GC-MS 6800 GC / MS appearance
2. Experimental part
2.1 Test principle
分析，依据目标化合物的保留时间和特征离子定性，用外标法定量。 Tobacco samples were accurately weighed after being shredded, and ultrasonically extracted with ethyl acetate, an organic solvent. The extracts were filtered, analyzed by GCMS , and quantified by external standard methods based on the retention time and characteristic ions of the target compounds.
2.2 Main instruments and equipment, consumables and reagents
GC-MS 6800 Gas Chromatograph Mass Spectrometer with Electron Impact Source (Jiangsu Tianrui Instrument Co., Ltd.)
（国家标准物质网）； Nicotine Standard: 99% purity (National Standards Network);
级（默克集团）； Ethyl acetate: HPLC grade (Merck Group);
（空气化工） Helium: 99.999% (air chemical)
2.3 Instrument test conditions
， 30m × 0.25mm × 0.25 μ m ； Column: Agilent DB-5 , 30m × 0.25mm × 0.25 μm;
℃， 20 ℃ /min升至280 ℃保持3min ； Oven program temperature rising conditions: initial temperature 100 ℃, 20 ℃ / min to 280 ℃ for 3min ;
： 1 ； Injection method: split injection, split ratio 10 : 1 ;
℃； Inlet temperature: 280 ℃;
℃； Temperament interface temperature: 280 ℃;
℃； Ion source temperature: 260 ℃;
，流速1.0mL/min ； Carrier gas: Helium, purity ≥ 99.999% , flow rate 1.0mL / min ;
； Ionization mode: EI ;
； Ionization energy: 70eV ;
Solvent removal time: 3min
（ FULL SCAN ）定性（扫描范围： 45-200amu ）， SIM模式定量。 Measurement method: TIC ( FULL SCAN ) qualitative (scanning range: 45-200amu ), SIM mode quantitative.
3. Test results
3.1 Qualitative results of the two target components
尼古丁质谱图 Figure 2. Nicotine mass spectrum
尼古丁总离子流图 Figure 3. Nicotine total ion chromatogram
目标物基本测试信息 Table 1. Basic test information of the target
号 CAS number
84 * 133 161 162
3.2 Sample test
线性良好。 The target has good linearity from 5ppm to 100ppm . The low-level nicotine was spiked, and the sample was subjected to ultrasonic extraction with ethyl acetate. 加标水平下谱图如下，得到了比较满意的效果。 The spectrum at the 50 ppm fortified level is as follows, and relatively satisfactory results were obtained.
加标SIM图 Figure 4. 350ppm Spike SIM
，在SIM扫描模式下进行测试，方法稳定可靠，线性范围好，灵敏度高，受杂质峰的干扰小，可以对烟草中的尼古丁进行有效的定性和定量分析。 This experiment uses GC-MS 6800 and is tested in SIM scan mode. The method is stable and reliable, has a good linear range, high sensitivity, and is less affected by impurity peaks. It can effectively analyze the nicotine in tobacco.
 GB / T 23355-2009 Determination of nicotine in total particulate phase of cigarettes Gas chromatography