Method for preparing tomato seed oil rich in high cis-lycopene
Through the combined use of steam expansion and subcritical extraction technology, the problem of low cis lycopene content in tomato seed oil in the existing technology has been solved, and the nutritional value and functional characteristics of tomato seed oil have been improved, and it is suitable for industrial production.
Patent Information
- Application Number
- CN202510467944.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-15
- Publication Date
- 2025-07-04
AI Technical Summary
The prior art is difficult to efficiently increase the content and proportion of cis-lycopene in tomato seed oil. Chemical methods have by-product residues and complex processes, and the physical field technology is low and the cost is high.
The combination of steam expansion and subcritical extraction technology is used to destroy the cell wall of tomato seeds by high temperature and high pressure to promote the release of lycopene and the transformation of trans to cis isomers, and extraction is performed using butane as a solvent under mild conditions.
It significantly increases the content and proportion of cis lycopene in tomato seed oil, reduces the proportion of trans lycopene, enhances nutritional value and functional characteristics, and is suitable for industrial production.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of food processing and functional oil development, and more specifically, to a method for preparing tomato seed oil rich in high-cis lycopene. Background Art
[0002] Tomato seeds are rich in 20 - 36% oil, which has health benefits such as preventing cardiovascular diseases. The extraction of tomato seed oil can reduce waste, increase processing added value, and provide diverse edible oil options. In 2014, tomato seed oil was listed as a new food raw material by the Food Safety Law of the People's Republic of China and the Administrative Measures for the Safety Review of New Food Raw Materials, and thus entered the market as a new type of functional vegetable oil.
[0003] Lycopene is a carotenoid with strong antioxidant activity. Its cis isomers have higher biological activity and absorption efficiency compared to the trans isomers. However, lycopene in natural tomato seed oil mainly exists in the trans configuration (accounting for more than about 80%), and the content of cis isomers is extremely low. In the prior art, chemical methods (such as acid catalysis) or thermal processing can induce cis isomerization, but there are problems such as by-product residues, nutrient loss, and complex processes. In recent years, physical field technologies (such as ultrasonic waves, microwaves, high-pressure homogenization) have been used to promote the transformation of natural components, but there are few studies on the cis isomerization of lycopene, and there are defects such as low efficiency and high cost.
[0004] Therefore, providing a method for preparing tomato seed oil rich in high-cis lycopene is an urgent problem to be solved by those skilled in the art. Summary of the Invention
[0005] In view of this, the present invention provides a method for preparing tomato seed oil rich in high-cis lycopene. This method uses the combined technology of steam explosion and subcritical extraction to effectively promote the cis isomerization of lycopene in tomato seed oil, aiming to increase the total content and proportion of cis-lycopene in tomato seed oil. This method is not only simple and efficient in operation, but also can significantly improve the nutritional value and functional properties of tomato seed oil, providing a new technical path for the development of high-value-added functional foods and health products.
[0006] To achieve the above object, the present invention adopts the following technical scheme:
[0007] A method for preparing tomato seed oil rich in high-cis lycopene, comprising the following steps:
[0008] (1) Steam explosion treatment: Weigh clean tomato seeds and add them to the material bin of the steam explosion equipment. Introduce saturated water steam. The explosion pressure is selected to be 0.8 - 1.2 MPa, the pressure holding time is 30 s, and the pressure reduction is terminated within an extremely short time. Then, systematically collect and dry the tomato seeds after steam explosion treatment, and cool them to room temperature. Next, crush the tomato seeds cooled to room temperature and sieve them through a 20 - 80 mesh sieve.
[0009] (2) Subcritical butane extraction: The dosage ratio of the crushed tomato seeds sieved through a 20 - 80 mesh sieve to n - butane is 1:8 - 12 g / mL, the extraction temperature is 40 - 60 °C, and the extraction time is 15 - 75 min. After extraction, centrifuge to obtain tomato seed oil rich in high - cis lycopene.
[0010] Furthermore, the drying in step (1) is drying in an oven at a temperature of 40 - 60 °C.
[0011] Furthermore, the centrifugation in step (2) is centrifuging in a centrifuge at a rotational speed of 5000 - 8000 rpm for 20 - 30 min.
[0012] As can be seen from the above - mentioned technical solutions, compared with the prior art, the present invention discloses a method for preparing tomato seed oil rich in high - cis lycopene. The tomato seed raw materials are sequentially subjected to steam explosion treatment and subcritical extraction to obtain tomato seed oil rich in high - cis lycopene. The steam explosion treatment destroys the cell wall of tomato seeds under high - temperature and high - pressure conditions, promotes the release of lycopene and the conversion of trans - to cis - isomers. The subcritical extraction uses butane as a solvent under mild conditions to efficiently extract lycopene and maximize the retention of its biological activity and cis - structure. The present invention combines the steam explosion treatment and subcritical extraction technology, significantly improving the content and proportion of cis - lycopene in tomato seed oil, while reducing the proportion of trans - lycopene, thereby enhancing the nutritional value and functional properties of tomato seed oil. After adopting this technology, the content of cis - lycopene in tomato seed oil increases significantly, and the functional properties are significantly improved. The method for preparing tomato seed oil rich in high - cis lycopene of the present invention is simple in operation, low in cost, and suitable for industrial production. Specific Embodiments
[0013] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
[0014] Determination of lycopene: Weigh 0.5 g of tomato seed oil, dissolve it with chromatographic grade ethyl acetate, and make up the volume to 10 mL. Manually shake it for 30 s and filter it through a 0.22 μm organic filter membrane; Separation and detection are carried out by high performance liquid chromatography - diode array detector (HPLC - PDA), and qualitative identification is carried out according to the retention time and spectral characteristics.
[0015] Detection conditions: Waters YMC C30 column (4.6 mm x 250 mm, 5 μm), column temperature 30 °C. Mobile phase A consists of 88% methanol, 5% methyl tert - butyl ether (MTBE) and 7% water; Mobile phase B consists of 80% MTBE and 20% methanol; Flow rate is 1 mL / min, detection wavelength is 471 nm; Injection volume: 0.02 mL; DAD spectral scanning range: 200 nm - 600 nm.
[0016] Example 1
[0017] Weigh 1000 g of clean tomato seeds and add them to the material bin of the steam explosion equipment (QBS - 200). Pass in saturated steam, select the explosion pressure to be 0.8 MPa, the pressure - maintaining time is 30 s, and decompress and terminate in a very short time (0.0875 s) to achieve steam explosion; Systematically collect the tomato seeds after steam explosion treatment, place them in an oven at 60 °C for drying, and cool them to room temperature.
[0018] Crush the above - mentioned tomato seeds and pass them through an 80 - mesh sieve, and then extract them with sub - critical butane; The extraction ratio of tomato seeds to n - butane is 1:8 (g / mL), the extraction temperature is 40 °C, and the reaction time is 45 min. Carry out extraction under these conditions;
[0019] After extraction, centrifuge in a centrifuge at 8000 rpm for 30 min, and finally obtain tomato seed oil extracted by the combination of steam explosion and sub - critical extraction; The detection method of lycopene is separation and detection by high performance liquid chromatography - diode array detector (HPLC - PDA).
[0020] Example 2
[0021] Weigh 1000 g of clean tomato seeds and add them to the material bin of the steam explosion equipment (QBS - 200). Pass in saturated steam, select the explosion pressure to be 1.0 MPa, the pressure - maintaining time is 30 s, and decompress and terminate in a very short time (0.0875 s) to achieve steam explosion; Systematically collect the tomato seeds after steam explosion treatment, place them in an oven at 40 °C for drying, and cool them to room temperature.
[0022] The above tomato seeds are crushed and then screened through a 40-mesh sieve, and then extracted with subcritical butane; the extraction ratio of tomato seeds to n-butane is 1:10 (g / mL), the extraction temperature is 60 °C, and the reaction time is 60 min. Extraction is carried out under these conditions;
[0023] After extraction, centrifuge for 20 min in a centrifuge at a speed of 6000 rpm, and finally obtain tomato seed oil extracted by the combined use of steam explosion and subcritical extraction; the detection method of lycopene is separation and detection by high performance liquid chromatography-diode array detector (HPLC-PDA).
[0024] Example 3
[0025] Weigh 1000 g of clean tomato seeds and add them to the material bin of the steam explosion equipment (QBS-200), introduce saturated steam, select the explosion pressure to be 1.2 MPa, the pressure holding time is 30 s, and terminate the pressure reduction in a very short time (0.0875 s) to achieve steam explosion; systematically collect the tomato seeds after steam explosion treatment, place them in an oven at 50 °C for drying, and cool to room temperature.
[0026] The above tomato seeds are crushed and then screened through a 20-mesh sieve, and then extracted with subcritical butane; the extraction ratio of tomato seeds to n-butane is 1:12 (g / mL), the extraction temperature is 50 °C, and the reaction time is 15 min. Extraction is carried out under these conditions;
[0027] After extraction, centrifuge for 25 min in a centrifuge at a speed of 7000 rpm, and finally obtain tomato seed oil extracted by the combined use of steam explosion and subcritical extraction; the detection method of lycopene is separation and detection by high performance liquid chromatography-diode array detector (HPLC-PDA).
[0028] Comparative Example 1
[0029] Weigh 1000 g of clean tomato seeds and add them to the material bin of the steam explosion equipment (QBS-200), introduce saturated steam, select the explosion pressure to be 0.2 MPa, the pressure holding time is 30 s, and terminate the pressure reduction in a very short time (0.0875 s) to achieve steam explosion; systematically collect the tomato seeds after steam explosion treatment, place them in an oven at 60 °C for drying, and cool to room temperature.
[0030] The above tomato seeds are crushed and then screened through a 40-mesh sieve, and then extracted with subcritical butane; the extraction ratio of tomato seeds to n-butane is 1:10 (g / mL), the extraction temperature is 60 °C, and the reaction time is 50 min. Extraction is carried out under these conditions;
[0031] After extraction, centrifuge at 5000 rpm for 30 min in a centrifuge to finally obtain tomato seed oil extracted by the combined use of steam explosion and subcritical extraction; the detection method of lycopene is separation and detection by high performance liquid chromatography - diode array detector (HPLC - PDA).
[0032] Comparative Example 2
[0033] Weigh 1000 g of clean tomato seeds and add them to the material bin of the steam explosion equipment (QBS - 200). Introduce saturated steam, select the explosion pressure to be 0.4 MPa, the pressure - maintaining time to be 30 s, and terminate the pressure reduction within an extremely short time (0.0875 s) to achieve steam explosion; systematically collect the tomato seeds after steam explosion treatment, place them in an oven at 60 °C for drying, and cool to room temperature.
[0034] Crush the above - mentioned tomato seeds and sieve them through a 60 - mesh sieve, and then extract with subcritical butane; the extraction ratio of tomato seeds to n - butane is 1:8 (g / mL), the extraction temperature is 40 °C, and the reaction time is 50 min. Carry out extraction under these conditions.
[0035] After extraction, centrifuge at 5000 rpm for 30 min in a centrifuge to finally obtain tomato seed oil extracted by the combined use of steam explosion and subcritical extraction; the detection method of lycopene is separation and detection by high performance liquid chromatography - diode array detector (HPLC - PDA).
[0036] Comparative Example 3
[0037] Weigh 1000 g of clean tomato seeds and add them to the material bin of the steam explosion equipment (QBS - 200). Introduce saturated steam, select the explosion pressure to be 0.6 MPa, the pressure - maintaining time to be 30 s, and terminate the pressure reduction within an extremely short time (0.0875 s) to achieve steam explosion; systematically collect the tomato seeds after steam explosion treatment, place them in an oven at 60 °C for drying, and cool to room temperature.
[0038] Crush the above - mentioned tomato seeds and sieve them through a 60 - mesh sieve, and then extract with subcritical butane; the extraction ratio of tomato seeds to n - butane is 1:10 (g / mL), the extraction temperature is 45 °C, and the reaction time is 60 min. Carry out extraction under these conditions.
[0039] After extraction, centrifuge at 5000 rpm for 30 min in a centrifuge to finally obtain tomato seed oil extracted by the combined use of steam explosion and subcritical extraction; the detection method of lycopene is separation and detection by high performance liquid chromatography - diode array detector (HPLC - PDA).
[0040] Comparative Example 4
[0041] The tomato seed oil was prepared according to the method of Example 1, with the difference from Example 1 being that the tomato seeds were not subjected to steam explosion treatment.
[0042] The tomato seeds were dried in an oven at 60 °C and cooled to room temperature. The above-mentioned tomato seeds were crushed and passed through a 60-mesh sieve, and then extracted with subcritical butane; the extraction ratio of tomato seeds to n-butane was 1:8 (g / mL), the extraction temperature was 40 °C, and the reaction time was 45 min. Extraction was carried out under these conditions;
[0043] After extraction, centrifugation was carried out in a centrifuge at 5000 rpm for 30 min, and finally subcritically extracted tomato seed oil was obtained; the detection method for lycopene was separation and detection using high performance liquid chromatography - diode array detector (HPLC - PDA).
[0044] Comparative Example 5
[0045] Weigh 1000 g of clean tomato seeds and add them to the material bin of the steam explosion equipment (QBS - 200). Saturated steam was introduced, the explosion pressure was selected to be 1.0 MPa, the pressure holding time was 30 s, and decompression was terminated within an extremely short time (0.0875 s) to achieve steam explosion; the tomato seeds after steam explosion treatment were systematically collected, placed in an oven at 60 °C for drying, and cooled to room temperature.
[0046] The above-mentioned tomato seeds were pressed for oil production using a screw press. After pressing, centrifugation was carried out in a centrifuge at 5000 rpm for 30 min, and finally tomato seed oil produced by the combination of steam explosion and pressing (with a relatively low oil yield) was obtained; the detection method for lycopene was separation and detection using high performance liquid chromatography - diode array detector (HPLC - PDA).
[0047] The lycopene detection results of Examples 1 - 3 and Comparative Examples 1 - 5 are shown in Table 1.
[0048] Table 1 Analysis of lycopene content in tomato seed oil prepared in Examples 1 - 3 and Comparative Examples 1 - 5 (mg / kg)
[0049]
[0050] The results in Table 1 show that in Comparative Example 1, the total cis - proportion of lycopene is the lowest; Examples 1 - 3 and Comparative Examples 1 - 3 indicate that steam explosion treatment can promote the isomerization of lycopene in tomato seed oil, among which in Example 2, the total cis - proportion is the highest at 72.839% under a pressure of 1.0 MPa. The cis - isomerization effect is significant, and tomato seed oil rich in cis - lycopene is successfully obtained. In addition, in Comparative Example 4, the sample was not subjected to steam explosion treatment, and the total cis - proportion reached 52.267%, which is significantly lower than 72.893%.
[0051] For Comparative Example 5 and Example 2, after steam explosion treatment at 1.0 MPa, pressing extraction and subcritical extraction were respectively used; it can be seen from Table 1 that for Example 2 (subcritical extraction): the total cis proportion was 72.893%, and the total cis amount was 97.700 mg / kg; for Comparative Example 5 (pressing extraction): the total cis proportion was 55.773%, and the total cis amount was 33.686 mg / kg. Under the same steam explosion treatment at 1.0 MPa, the subcritical extraction method better retained the lycopene component than the pressing extraction method, and the contents of each cis-lycopene increased significantly.
[0052] The sterol contents of the tomato seed oils prepared in Example 2 and Comparative Examples 1-4 are shown in Table 2.
[0053] Table 2 Sterol contents (mg / kg) of the tomato seed oils prepared in Example 2 and Comparative Examples 1-4
[0054]
[0055] The results in Table 2 show that steam explosion increased the sterol content in tomato seed oil. The total sterol content of Example 2 was significantly higher than that of Comparative Examples 1-3. Its advantage mainly stemmed from the increase in the contents of δ5-avenasterol and δ7-stigmastenol. At the same time, β-sitosterol and stigmasterol also remained at relatively high levels, and the component distribution was balanced.
[0056] The tocopherol and total phenol contents of the tomato seed oils prepared in Example 2 and Comparative Examples 1-4 are shown in Table 3.
[0057] Table 3 Tocopherol and total phenol contents (mg / kg) of the tomato seed oils prepared in Example 2 and Comparative Examples 1-4
[0058] α-tocopherol γ-tocopherol total tocopherol total phenol Example 2 128.569 997.614 1126.182 161.284 Comparative Example 1 93.976 856.245 950.221 44.327 Comparative Example 2 102.369 918.015 1020.384 74.245 Comparative Example 3 105.860 932.600 1038.460 100.565
[0059] The results in Table 3 show that Example 2 was significantly superior to Comparative Examples 1-3 in terms of the contents of α-tocopherol (128.569), γ-tocopherol (997.614), total tocopherol (1126.182), and total phenol (161.284), indicating that steam explosion (1.0 MPa) could more effectively retain or enrich tocopherols and phenolic substances.
[0060] In summary, the combination of steam explosion treatment and subcritical extraction can not only promote the cis-isomerization of lycopene in tomato seed oil, but also facilitate the easy dissolution of fat-soluble components in oilseeds. Through steam explosion treatment, the cell structure of tomato seeds was effectively destroyed, releasing more lycopene and promoting the conversion of trans-lycopene to cis-isomers under high temperature and high pressure conditions. At the same time, the subcritical extraction technology further optimized the extraction efficiency and ensured the efficient enrichment of cis-lycopene.
[0061] This combined process not only significantly increases the content and proportion of cis-lycopene as well as other fat-soluble nutrients, but also reduces the proportion of trans-lycopene, thereby enhancing the nutritional value and functional properties of tomato seed oil. Future research can further optimize the process parameters and explore its application potential in the fields of functional foods and health products.
[0062] The above description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to the broadest scope consistent with the principles and novel features disclosed herein.
Claims
1. A method for preparing tomato seed oil rich in high-cis lycopene, characterized in that, Including the following steps: (1) Steam explosion treatment: Weigh clean tomato seeds and add them to the material bin of the steam explosion equipment. Pass in saturated water vapor. The explosion pressure is selected to be 0.8 - 1.2 MPa, the pressure maintenance time is 30 s, and the pressure reduction is terminated within an extremely short time. Then, systematically collect and dry the tomato seeds after steam explosion treatment, and cool them to room temperature. Next, crush the tomato seeds cooled to room temperature and sieve them through a 20 - 80 mesh sieve; (2) Subcritical butane extraction: The dosage ratio of the tomato seeds sieved through a 20 - 80 mesh sieve after crushing to n - butane is 1:8 - 12 g / mL, the extraction temperature is 40 - 60 °C, and the extraction time is 15 - 75 min. After extraction, centrifuge to obtain tomato seed oil rich in high - cis lycopene.
2. A method for preparing tomato seed oil rich in high-cis lycopene according to claim 1, characterized in that, The drying in step (1) is drying in an oven at a temperature of 40 - 60 °C.
3. A method for preparing tomato seed oil rich in high-cis lycopene according to claim 1, characterized in that, The centrifugation in step (2) is centrifuging in a centrifuge at a rotation speed of 5000 - 8000 rpm for 20 - 30 min.