气相色谱法测定烟用香精中的乙醇、1,2-丙二醇和丙三醇

doi:10.3969/j.issn.1001-1803.2019.05.012

摘要/Abstract

摘要：

为了准确测定烟用香精中溶剂的含量,以1,4-丁二醇为内标建立了检测烟用香精中乙醇、1,2-丙二醇和丙三醇的气相色谱法,采用该方法测定了30个烟用香精样品。结果表明：该方法的检出限和定量限范围在0.019~0.088和0.063~0.293 g/L之间;回收率在97.5%~101.6%之间;相对标准偏差（RSD）为0.61%~0.89%。所测样品中均检出1,2-丙二醇,均未检出丙三醇;13个样品中检测出乙醇。该方法前处理简单、灵敏度高、定性定量准确,适用于烟用香精中乙醇、1,2-丙二醇和丙三醇的定性定量分析。

关键词: 烟用香精, 乙醇, 1,2-丙二醇, 丙三醇, 气相色谱法

Abstract:

In order to accurately determine the content of solvents in tobacco flavors, a gas chromatography method was developed for the determination of ethanol, 1,2-propylene glycol and glycerol in tobacco flavor using 1,4-butanediol as an internal standard. Thirty tobacco flavor samples were tested by this method. Results show that the limit of detection and limit of quantitation are 0.019-0.088 and 0.063-0.293 g/L, respectively. The recoveries are 97.5%-101.6% with the relative standard deviations（RSD）ranging from 0.61% to 0.89%. 1,2-propylene glycol is detected, while glycerol is not detected in all samples; ethanol is detected in thirteen samples. This method has the advantages of simple pretreatment, high sensitivity and high accuracy, and is suitable for the determination of ethanol, 1,2-propylene glycol and glycerol in tobacco flavor.

Key words: tobacco flavor, ethanol, 1,2-propylene glycol, glycerol, gas chromatography

中图分类号:

TQ655

肯生叶,李峰,饶国华,段勤,杨雪燕,邹由. 气相色谱法测定烟用香精中的乙醇、1,2-丙二醇和丙三醇[J]. 日用化学工业, 2019, 49(5): 346-350.

KEN Sheng-ye,LI Feng,RAO Guo-hua,DUAN Qin,YANG Xue-yan,ZOU You. Determination of ethanol, 1, 2-propylene glycol and glycerol in tobacco flavor with gas chromatography method[J]. China Surfactant Detergent & Cosmetics, 2019, 49(5): 346-350.

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参考文献 17

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提取时间/min	w（乙醇）/ %	w（1,2-丙二醇）/ %	w（丙三醇）/ %
5	15.35	44.86	24.18
10	15.64	44.82	24.52
15	15.44	44.46	24.43
20	15.52	44.85	24.25
25	15.40	44.71	25.59
平均值	15.47	44.74	24.39
RSD/%	0.7	0.4	0.7

称样量/mg	w（乙醇）/ %	w（1,2-丙二醇）/ %	w（丙三醇）/ %
100	15.44	44.34	24.65
150	15.25	44.60	24.30
200	15.43	44.88	24.40
300	15.50	44.64	24.50
400	15.30	44.38	24.30
500	15.17	44.24	24.29
平均值	15.35	44.51	24.41
RSD/%	0.8	0.5	0.6

化合物	回归方程	相关系数	检出限/（g·L^-1）	定量限/（g·L^-1）
乙醇	y=0.940 2x-0.035 2	0.999 9	0.050	0.167
1,2-丙二醇	y=0.823 9x-0.052 5	0.999 9	0.019	0.063
丙三醇	y=0.577 1x-0.161 3	0.999 7	0.088	0.293

化合物	萃取液质量浓度/（g·L^-1）	加标量/（g·L^-1）	检测质量浓度/（g·L^-1）	回收率/%
乙醇	3.13	1.6	4.69	97.50
		3.2	6.31	99.38
		4.8	7.81	97.50
1,2-丙二醇	8.91	4.52	13.49	101.33
		9.04	17.86	99.00
		13.56	22.19	97.94
丙三醇	5.04	2.5	7.58	101.60
		5.0	9.98	98.80
		7.5	12.62	101.07

样品编号	本方法		标准方法
样品编号	w（乙醇）/ %	w（1,2-丙二醇）/%	w（乙醇）/ %	w（1,2-丙二醇）/%
1#	—	75.62	—	76.91^*
2#	1.77	73.70	2.00	75.98^*
3#	—	94.28	—	95.48^*
4#	—	94.32	—	92.54^*
5#	2.00	93.24	1.90	93.90^*
6#	—	88.65	—	89.18^*
7#	—	31.92	—	24.40
8#	—	77.71	—	78.66^*
9#	—	37.62	—	27.25
10#	—	70.54	—	69.34^*
11#	0.84	54.31	—	52.59
12#	1.08	31.60	—	30.71
13#	—	71.70	—	71.08^*
14#	—	38.36	—	30.04
15#	—	82.24	—	81.02^*
16#	—	66.89	—	67.37
17#	9.06	83.73	8.50	82.72^*
18#	1.32	93.84	1.45	93.17^*
19#	—	73.70	—	70.93^*
20#	1.52	92.67	1.58	91.81^*
21#	10.94	77.08	10.75	77.70^*
22#	1.22	87.60	—	88.14^*
23#	—	32.25	—	25.50
24#	—	43.66	—	44.96
25#	4.84	77.12	4.59	77.92^*
26#	—	81.12	—	81.73^*
27#	44.48	51.27	42.97	50.97
28#	30.97	65.79	29.78	66.55^*
29#	—	7.23	—	6.62
30#	42.43	46.52	43.20	46.49