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Method for removing safrole from myristica oil

A technology of nutmeg oil and safrole, which is applied in the direction of essential oil/perfume, fat production, etc., can solve the problems of spices that do not meet industrial production and have economic application value, cumbersome preparation process, high synthesis cost, etc., and achieve Improved safety and application range, simple process and low cost

Inactive Publication Date: 2017-06-20
广州华芳烟用香精有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Using the molecularly imprinted copolymer, repeated adsorption and elution of nutmeg oil can remove up to 97% of safrole in the nutmeg oil sample, but the material preparation process of this method is cumbersome and the synthesis cost is high
[0006] At present, there is no report on the selective removal of safrole from nutmeg oil samples in China, and the fragrance industry has not yet had a removal method that meets industrial production and has economic application value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Carry out molecular distillation and separation of nutmeg oil, control the temperature at 30°C, and vacuum at 100Pa, collect light component 1# and heavy component 2# respectively;

[0020] (2) Carry out silica gel column chromatography with the heavy component 2# that is rich in safrole in step (1), adopt mixed solvent to rinse, collect the eluent without safrole, remove solvent and do not have safrole in step (1) The light component 1# is mixed to obtain the nutmeg oil from which safrole has been removed, wherein the silica gel mesh used is 100-200 mesh, and the mixed solvent is V 石油醚 :V 乙酸乙酯 =15:1 uniformly mixed solvent, the boiling point of petroleum ether used is 60~90°C;

[0021] (3) The above samples were taken and detected by gas chromatography-mass spectrometry, and the safrole in the nutmeg oil was reduced from the original 13583.59ug / g to 0.29ug / g.

Embodiment 2

[0023] (1) Carry out molecular distillation and separation of nutmeg oil, control the temperature at 40°C, and vacuum at 300Pa, collect light component 1# and heavy component 2# respectively;

[0024] (2) Carry out silica gel column chromatography with the heavy component 2# that is rich in safrole in step (1), adopt mixed solvent to rinse, collect the eluent without safrole, remove solvent and do not have safrole in step (1) The light component 1# is mixed to obtain the nutmeg oil from which safrole has been removed, wherein the silica gel mesh used is 200-300 mesh, and the mixed solvent is V 正己烷 :V 乙酸乙酯 = 10:1 uniformly mixed solvent;

[0025] (3) The above samples were taken and detected by gas chromatography-mass spectrometry, and the safrole in the nutmeg oil was reduced from the original 15938.74ug / g to 0.37ug / g.

Embodiment 3

[0027] (1) Carry out molecular distillation and separation of nutmeg oil, control the temperature at 50°C, and vacuum at 500Pa, collect light component 1# and heavy component 2# respectively;

[0028] (2) Carry out silica gel column chromatography with the heavy component 2# that is rich in safrole in step (1), adopt mixed solvent to rinse, collect the eluent without safrole, remove solvent and do not have safrole in step (1) The light component 1# is mixed to obtain the nutmeg oil from which safrole has been removed, wherein the silica gel mesh used is 300-400 mesh, and the mixed solvent is V 6号溶剂 :V 乙酸乙酯 = 8:1 uniformly mixed solvent;

[0029] (3) The above samples were taken and detected by gas chromatography-mass spectrometry, and the safrole in the nutmeg oil was reduced from the original 11353.41ug / g to 0.33ug / g.

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Abstract

The invention provides a method for removing safrole from myristica oil. The method comprises the following steps: separating commercially available myristica oil serving as a raw material through molecular distillation, obtaining a safrole-free light component 1# and a safrole-enriched heavy component 2#, further carrying out silica gel chromatography on the heavy component 2#, carrying out leaching through a nonpolar solvent and ethyl acetate mixed solution, collecting safrole-free eluant, removing a solvent from the safrole-free eluant, and mixing the solvent-removed safrole-free eluant with the safrole-free light component 1#, thus obtaining the safrole-removed myristica oil. According to the method for removing the safrole from the myristica oil, the safrole in the myristica oil can be effectively removed, and the content of the safrole in the refined myristica oil is less than 1 mug / g, and the product safety and the application range are substantially improved. A preparation method is simple in operation process, low in cost and suitable for industrial production.

Description

technical field [0001] The invention relates to a process for removing safrole from nutmeg oil, which belongs to the technical field of spice finishing. Background technique [0002] Nutmeg is the dry mature seed kernel of Myristica fragrans Houtt, also known as nutmeg and cardamom. Distributed in Indonesia, Malaysia, West Indies, Brazil and other places. my country Taiwan, Guangdong, Yunnan and other places have introduced cultivated products. Nutmeg is warm in nature, pungent and slightly bitter, and has the effects of warming the middle and promoting qi, astringent intestines and antidiarrheal. It has been widely used in traditional Chinese medicine for thousands of years to treat gastrointestinal diseases such as diarrhea and vomiting. Previous studies have shown that its seeds contain various components such as volatile oil, fatty oil and protein. The volatile oil mainly includes myristicin, terpinen-4-ol, γ-terpinene, α-pinene, β-pinene, limonene, elemene, eugenol, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C11B9/00
Inventor 卢真保黄艳孙胜南胡武林德洪赵世兴周叶燕陈志雄王学娟郑作略
Owner 广州华芳烟用香精有限公司
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