Grass ear shaft essential oil and extraction method thereof

Abstract

The invention provides a composition of grass ear shaft essential oil and an extraction method of the grass ear shaft essential oil. A steam distillation method is adopted to extract the amomum tsao-ko spike stalk essential oil from crushed amomum tsao-ko spike stalks, when fresh amomum tsao-ko spike stalks are adopted to extract the amomum tsao-ko spike stalk essential oil, the mass ratio of the amomum tsao-ko spike stalks to water is 1: 1-1: 4, and the amomum tsao-ko spike stalks and water can be directly subjected to steam distillation after being mixed and can also be soaked for 30-60 minutes; when the dry amomum tsao-ko spike stalks are used for extracting the amomum tsao-ko spike stalks, the mass ratio of the amomum tsao-ko spike stalks to water is 1: 8-1: 10, the amomum tsao-ko spike stalks need to be soaked for 30-90 minutes, and then steam distillation is performed; the steam distillation time is 2-5 hours; when the fresh amomum tsao-ko spike stalks are used for extracting the amomum tsao-ko spike stalk essential oil, the oil yield is 0.03%-0.15%; when the extract is used for extracting the amomum tsao-ko spike stalk essential oil from the amomum tsao-ko spike stalk, the oil yield is 0.24-0.96%. The amomum tsao-ko spike-stalk essential oil is prepared from the following main components: 1, 8-cineole, beta-pinene, trans-nerolidol, alpha-pinene, linalool, beta-cineole, delta-junifolene, limonene, neraldehyde, alpha-terpilenol and ocimene.

Description

Technical Field

[0001] The invention relates to an essential oil and an extraction method thereof, more specifically to an essential oil of tsaoko spike cob and an extraction method thereof. Background Art

[0002] Tsao-ko (Amomum tsao-ko Crevost et Lemaire) is a perennial herbaceous plant of the ginger family, the genus Cardamom. Its fruit (commonly known as tsao-ko) grows on an upright spike axis about 20-30 cm long above the ground near the roots. When people harvest tsao-ko, they harvest the tsao-ko spike axis together with the tsao-ko (similar to a bunch of grapes), transport the whole bunch of tsao-ko from the mountain to a collection point at the foot of the mountain, and then pick the tsao-ko from the tsao-ko spike. The tsao-ko is transported to a processing point for processing, and the tsao-ko spike axis is discarded as garbage (see Figure 1 ). 90% of my country's cardamom is produced in Yunnan Province, and the main planting area in Yunnan Province is Nujiang Prefecture, with production and planting area accounting for more than 55% of the country. At present, the cardamom planting area in Nujiang Prefecture has reached 1.1145 million mu, and the annual output of fresh fruit is more than 30,000 tons. From the quality point of view, in a bunch of cardamom, cardamom spikes account for about 10%. It can be seen that more than 5,000 tons of cardamom spikes are discarded every year in the country, resulting in a waste of resources. In addition, cardamom spikes piled together will mold and produce a certain odor, which also pollutes the environment to a certain extent.

[0003] In order to make full use of the cardamom cob resources and promote local economic development, the present invention aims to provide a cardamom cob essential oil and a preparation method thereof, which can provide a theoretical basis for the deep processing and comprehensive utilization of the cardamom cob. Summary of the invention

[0004] Through research, the inventors found that the cardamom spike also contains aroma components (Wu Yajian, Liang Miao, Zhang Zhimin, Wang Rui, Liu Yuping*. Analysis of key aroma components in cardamom spikes treated with different enzymes [J]. Food Science, 2023, 44(12): 172-180.). The main aroma components in the cardamom spike are 1,8-cineole, β-pinene, γ-eucalyptol, linalool, trans-nerolidol, (E)-2-decenal, (E)-2-dodecenal, etc., which are close to the aroma component composition of the cardamom itself. Based on previous research, the inventors extracted the tsaoko cob essential oil from the tsaoko cob by steam distillation. Through aroma evaluation, it was found that the aroma of the tsaoko cob essential oil was close to that of the tsaoko essential oil. However, during the steam distillation process, part of the unsaturated fatty aldehydes such as (E)-2-decenal and (E)-2-dodecenal were dissolved in the distilled water, and part was oxidized into other components, which weakened the fatty aroma of the tsaoko cob. Therefore, it can be used not only for the preparation of edible flavors, but also for the preparation of daily flavors, and for flavoring products such as food, condiments, feed, and daily necessities.

[0005] The present invention provides an tsaoko cob essential oil and a preparation method thereof, which comprises:

[0006] (1) By comparing the mass spectrum data, retention index and aroma characteristics with those of the standard, the main components (content ≥ 2%) in the essential oil of the tsaoko cob were positively identified, wherein the main components (content, retention time) of the essential oil of the tsaoko cob in the present invention are 1,8-cineole (greater than 19%, retention time is 10.78min), β-pinene (greater than 8%, retention time is 8.22min), trans-nerolidol (greater than 4%, retention time is 33.31min), α-pinene (greater than 4%, retention time is 6.25min ), linalool (greater than 3%, retention time is 20.86min), β-eucalyptol (greater than 3%, retention time is 37.62min), δ-cadinene (greater than 3%, retention time is 26.94min), limonene (greater than 3%, retention time is 10.43min), neral (greater than 2%, retention time is 24.77min), α-terpineol (greater than 2%, retention time is 24.41min), ocimene (greater than 2%, retention time is 11.56min), and the content of other ingredients is less than 2%.

[0007] (2) The essential oil of the cardamom cob is obtained by extraction using a steam distillation method. The essential oil of the cardamom cob can be extracted from fresh cardamom cobs or dried cardamom cobs.

[0008] (3) When fresh cardamom cobs are used to extract cardamom cob essential oil, the mass ratio of cardamom cobs to water is 1:1 to 1:4. After the two are mixed, they can be directly steam distilled or soaked for 30 minutes to 60 minutes before steam distillation. When dry cardamom cobs are used to extract cardamom cob essential oil, the mass ratio of cardamom cobs to water is 1:8 to 1:10. They need to be soaked for 30 minutes to 90 minutes before steam distillation.

[0009] (4) The steam distillation time is 2h to 5h; when fresh grass fruit cobs are used to extract the grass fruit cob essential oil, the oil yield is 0.03% to 0.15%; when dry grass fruit cobs are used to extract the grass fruit cob essential oil, the oil yield is 0.24% to 0.96%.

[0010] (5) A gas chromatograph or gas chromatography-mass spectrometry equipped with a DB-Wax type (30m×0.25mmi.d.×0.25μm) capillary column was used to analyze the essential oil of the tsaoko spike cob. The injection port temperature was set to 240°C and the column heating program was as follows: the initial temperature was 35°C and maintained for 2 min; then the temperature was increased to 100°C at a rate of 6°C / min and maintained for 5 min; then the temperature was continued to be increased to 180°C at a rate of 5°C / min and maintained for 5 min; finally, the temperature was increased to 230°C at a rate of 6°C / min and maintained for 10 min.

[0011] The main advantages of the present invention are:

[0012] 1. The cardamom cobs discarded as garbage are used to extract cardamom cob essential oil, which turns waste into treasure and reduces pollution to the environment.

[0013] 2. Compared with other methods of extracting natural spices, the steam distillation method is simple. Farmers can customize appropriate equipment according to the actual yield of cardamom cobs and extract cardamom cob essential oil in their own yards. BRIEF DESCRIPTION OF THE DRAWINGS

[0014] Figure 1 Amomum villosum and amomum villosum spike cob.

[0015] Figure 2 Total ion chromatogram of gas chromatography-mass spectrometry analysis of Tsaoko cob essential oil. DETAILED DESCRIPTION

[0016] The present invention will be further described below in conjunction with the embodiments.

[0017] Example 1 Extraction of Tsaoko Spike Essential Oil from Dried Tsaoko Spike

[0018] Crush 100g of dry tsaoko cob and add it into a 2000mL single-mouth bottle, then add 900mL of deionized water into the single-mouth bottle and mix well. Place the single-mouth bottle containing tsaoko cob powder and water at room temperature for 30min, stirring every 10min. Then connect the steam distillation device, start timing when distillate starts to appear, perform steam distillation for 4h, collect the distillate, let it stand and centrifuge, and 0.24g of light yellow tsaoko cob essential oil can be obtained. Through the gas chromatograph analysis that DB-Wax type (30m×0.25mm id×0.25μm) capillary chromatographic column is housed, it is known that the essential oil contains 19.32% 1,8-cineole, 8.96% β-pinene, 4.53% trans-nerolidol, 4.08% α-pinene, 3.81% linalool, 3.77% β-cineole, 3.37% δ-cadinene, 3.30% limonene, 2.90% nerol, 2.65% α-terpineol and 2.38% ocimene.

[0019] Example 2 Extraction of Tsaoko Spike Essential Oil from Dried Tsaoko Spike

[0020] Crush 400g of dry tsaoko cob and add it into a 5000mL single-necked bottle, then add 3200mL of deionized water into the single-necked bottle and mix well. Place the single-necked bottle containing tsaoko cob powder and water at room temperature for 40min, stirring every 10min during the period. Then connect the steam distillation apparatus, start timing when distillate starts to appear, perform steam distillation for 5h, collect the distillate, let it stand and centrifuge, and 1.58g of light yellow tsaoko cob essential oil can be obtained. The analysis of the essential oil by a gas chromatograph equipped with a DB-Wax type (30m×0.25mm id×0.25μm) capillary column showed that the essential oil contained 20.12% 1,8-cineole, 9.05% β-pinene, 5.62% trans-nerolidol, 4.12% α-pinene, 4.23% linalool, 3.96% β-cineole, 3.69% δ-cadinene, 3.88% limonene, 3.12% nerol, 2.98% α-terpineol, and 2.67% ocimene.

[0021] Example 3 Extraction of Tsaoko Spike Essential Oil from Fresh Tsaoko Spike

[0022] Crush 500g of fresh tsaoko cob and add it into a 2000mL single-mouth bottle. Then add 1000mL of deionized water into the single-mouth bottle and mix well. Connect the steam distillation device and start timing when distillate starts to appear. Steam distill for 3.5h, collect the distillate, let it stand and centrifuge to obtain 0.52g of light yellow tsaoko cob essential oil. Through the gas chromatograph analysis that DB-Wax type (30m × 0.25mmi.d. × 0.25μm) capillary chromatographic column is housed, it is known that the essential oil contains 19.98% 1,8-cineole, 8.75% β-pinene, 4.88% trans-nerolidol, 4.67% α-pinene, 4.83% linalool, 3.18% β-cineole, 3.05% δ-cadinene, 4.12% limonene, 3.15% nerol, 2.82% α-terpineol and 2.54% ocimene.

[0023] Example 4 Extraction of Tsaoko Spike Essential Oil from Fresh Tsaoko Spike

[0024] 1000g of fresh tsaoko cob was crushed and added into a 5000mL single-necked bottle, and then 2500mL of deionized water was added into the single-necked bottle. After mixing evenly, the single-necked bottle containing tsaoko cob powder and water was placed at room temperature for 30min, during which time it was stirred every 10min. Then, a steam distillation device was connected, and the timing was started when distillate began to appear. The steam distillation was performed for 4.5h, and the distillate was collected. The distillate was allowed to stand and centrifuged to obtain 1.22g of light yellow tsaoko cob essential oil. Through the gas chromatograph analysis that DB-Wax type (30m × 0.25mmi.d. × 0.25μm) capillary chromatographic column is housed, it is known that the essential oil contains 21.05% 1,8-cineole, 8.63% β-pinene, 5.01% trans-nerolidol, 4.76% α-pinene, 4.79% linalool, 3.26% β-cineole, 3.19% δ-cadinene, 4.23% limonene, 3.25% nerol, 2.39% α-terpineol and 2.62% ocimene.

Claims

1. A kind of cardamom cob essential oil and its extraction method, it is characterized in that The essential oil of the tsaoko spike cob is extracted from the tsaoko spike cob. The components in the essential oil of the tsaoko spike cob whose content is greater than or equal to 2% through positive identification are composed of 1,8-cineole, β-pinene, trans-nerolidol, α-pinene, linalool, β-cineole, δ-cadinene, limonene, neral, α-terpineol and ocimene, and the content of other components is less than 1%.

2. When the essential oil of the tsaoko spike cob is extracted from the crushed fresh tsaoko spike cob by steam distillation, the mass ratio of the tsaoko spike cob to water is 1:1 to 1:

4. After the two are mixed, they can be directly steam distilled or soaked for 30min to 60min. The steam distillation time is 2h to 5h, and the oil yield is 0.03% to 0.15%.

3. When the essential oil of cardamom cob is extracted from the crushed dry cardamom cob by steam distillation, the mass ratio of cardamom cob to water is 1:8 to 1:10, and it needs to be soaked for 30 minutes to 90 minutes before steam distillation; the steam distillation time is 2 hours to 5 hours, and the oil yield is 0.24% to 0.96%.

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