高效分离杉木精油中柏木醇的研究

doi:10.3969/j.issn.0253-2417.2021.04.005

Abstract

Abstract:

The light and heavy components were preliminarily separated from the cedar oil by vacuum distillation technology, and then the cedrol was separated by the method of freezing crystallization. The cedrol content in the isolate was analyzed by GC/MS to determine the optimal process. By studying the effects of different reflux ratio and total reflux time in the vacuum distillation process on the content of cedrol in the collected fractions, the final determination of vacuum distillation conditions were 2-3 kPa, total reflux time for 1h, reflux ratio of 3-7, the highest mass fraction of cedrol was 97.89%, the recovery rate was 87.52%. The collected highest fraction of cedrol was dissolved in ethanol, and then frozen and crystallized, and the purity of cedrol was finally reached 98.43%, the recovery rate was 83.61%.

Key words: Chinese fir essential oil, vacuum distillation, frozen and crystallized, cedrol, efficient separation

CLC Number:

TQ35
R284.2

Jiechen PAN, Yichuan TANG, Chengjie SHU, Baojun SHI, Kai ZHU, Wei LI. High Efficient Separation of Cedrol from Chinese Fir Essential Oil[J]. Chemistry and Industry of Forest Products, 2021, 41(4): 29-34.

Figures/Tables 5

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References 17

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编号 No.	A 结晶温度/℃ crystallization temp.	B 乙醇体积分数/% volume fraction of ethanol	C 料液比(g∶mL) solid-to-solvent ratio	柏木醇纯度/% cedrol purity
1	5	90	1∶5	79.48
2	5	85	1∶4	70.41
3	5	80	1∶3	48.37
4	2	90	1∶4	65.12
5	2	85	1∶3	69.54
6	2	80	1∶5	47.95
7	0	90	1∶3	77.42
8	0	85	1∶5	75.55
9	0	80	1∶4	44.55
k₁	66.09	74.01	67.66
k₂	60.87	71.83	60.03
k₃	65.84	46.96	65.11
R	5.22	27.05	7.63

方差来源 source of source	离均差平方和¹⁾ sum of squares	自由度 d_f	均方 mean quare	F值 F value	p值 p value
修正的模型crrected model	1431.28^a	6	238.55	37.46	0.026
截距intercept	37428.06	1	37428.60	5877.08	0.000
A	39.28	2	19.64	3.08	0.245
B	1286.93	2	643.46	101.04	0.010
C	105.08	2	52.54	8.25	0.108
误差error	12.74	2	6.37
总和sum	38872.08	9

馏分序号 No.	塔顶温度/℃ temp. of tower top	馏分质量/g distillate weight	柏木醇质量分数/% mass fraction of cedrol	α-柏木烯质量分数/% mass fraction of α-cedrene
1	~100	9.0	2.23	13.62
2	100~110	14.7	1.62	24.83
3	110~130	141.4	3.03	49.43
4	130~140	51.4	20.92	27.49
5	140~148	97.0	70.84	3.81

项目 items		精馏时间/h distillation time	柏木醇馏分质量/g weight of cedrol	柏木醇质量分数/% mass fraction of cedrol	回收率/% recovery rate
全回流时间 total reflux time	20 min	5.0	84	56.64	42.52
	40 min	5.5	88	71.99	56.64
	60 min	6.0	97	70.84	61.44
馏分3回流比 fraction 3 reflux ratio	5∶1	6.1	108.0	65.20	65.20
馏分3回流比 fraction 3 reflux ratio	7∶1	6.5	99.0	93.38	85.60

编号 No.	柏木醇质量分数/% mass fraction of cedrol	回收率/% recovery rate
1	97.89	87.52
2	98.43	79.21
3	97.01	95.41

High Efficient Separation of Cedrol from Chinese Fir Essential Oil

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