Composite solubilizer and method for improving solubility of zanthoxylum oil resin in vegetable oil

Abstract

The invention discloses a composite solubilizer and a method for improving the solubility of zanthoxylum oil resin in vegetable oil, and belongs to the technical field of food processing. The composite solubilizer provided by the invention comprises linalool, sucrose acetate isobutyrate and propylene glycol. The zanthoxylum oil resin prepared by the composite solubilizer can achieve the effects of self stability and no precipitate or precipitate after being placed for a long time without removing pectin, and the zanthoxylum oil resin can be dissolved in vegetable oil in any proportion, so that the obtained zanthoxylum oil also has higher stability. Meanwhile, the method for improving the solubility of the zanthoxylum oil resin in the vegetable oil by using the composite solubilizer is simple in process and convenient to operate. Therefore, the composite solubilizer and the method for improving the solubility of the zanthoxylum oil resin in the vegetable oil have good industrial application prospects.

Description

Technical Field

[0001] This invention relates to the field of food processing technology, and more specifically, to a composite solubilizer and method for improving the solubility of pepper oleoresin in vegetable oils. Background Technology

[0002] Sichuan peppercorn( Zanthoxylum bungeanum Zanthoxylum bungeanum (Maxim.) is a deciduous small tree or perennial plant belonging to the Rutaceae family and the Zanthoxylum genus. It is also one of the most commonly used spices and seasonings in food processing.

[0003] Currently, food processing enterprises mainly use Sichuan pepper in the following ways: directly using crushed Sichuan pepper; extracting Sichuan pepper oil by soaking in vegetable oil; using Sichuan pepper aromatic oil obtained by steam distillation; and using Sichuan pepper oleoresin prepared by solvent extraction or supercritical CO2 extraction. Among these methods, Sichuan pepper oleoresin prepared by supercritical CO2 extraction has a flavor close to that of the original Sichuan pepper fruit, leaves no solvent residue, and has high safety, making it highly accepted by food processing enterprises. However, supercritical Sichuan pepper oleoresin has a high content of numbing substances and contains Sichuan pepper pectin, which easily aggregates and forms nuclei, promoting the crystallization of Sichuan pepper nuclein, resulting in precipitation and stratification, and making it unstable.

[0004] To address the aforementioned issues, some studies have focused on removing pectin from supercritical pecan oleoresin, including ethanol treatment and brine treatment. While the treated pecan oleoresin remains stable and does not readily precipitate, several problems persist: the precipitated pectin often contains flavor compounds such as pecan extract, leading to material waste; the process is complex; and precipitates are still generated again after adding edible vegetable oils such as soybean oil to the treated pecan oleoresin, causing inconvenience for downstream users.

[0005] In view of this, the present invention is proposed. Summary of the Invention

[0006] The purpose of this invention is to provide a composite solubilizer and method for improving the solubility of pepper oleoresin in vegetable oil. The pepper oleoresin prepared using this composite solubilizer is not only stable in its own state and does not precipitate or exudate after long-term storage, but it can also be dissolved in vegetable oil in any proportion, and the obtained pepper oil also has high stability and does not precipitate or exudate after long-term storage.

[0007] This invention is implemented as follows: In a first aspect, the present invention provides a composite solubilizer comprising: linalool, sucrose isobutyrate acetate, and propylene glycol.

[0008] Secondly, the present invention provides the application of the above-mentioned composite solubilizer in the preparation of products that improve the solubility of pepper oleoresin in vegetable oils.

[0009] Thirdly, the present invention provides a pepper oleoresin, comprising: the above-mentioned composite solubilizer, and pepper oleoresin extracted from pepper using supercritical carbon dioxide extraction technology.

[0010] Fourthly, the present invention provides a pepper oil comprising the aforementioned pepper oleoresin and vegetable oil.

[0011] Fifthly, the present invention provides a method for improving the solubility of Sichuan pepper oleoresin in vegetable oil, comprising: adding the above-mentioned composite solubilizer to Sichuan pepper oleoresin prepared by supercritical carbon dioxide extraction, mixing well, and then diluting it with vegetable oil to a target concentration.

[0012] The present invention has the following beneficial effects: This invention provides a composite solubilizer by combining linalool, sucrose isobutyrate acetate, and propylene glycol. The pectin in this composite solubilizer-prepared pepper oleoresin exhibits self-stability and shows no precipitation or exudation even after long-term storage without the need for pectin removal. Furthermore, this pepper oleoresin can be dissolved in vegetable oil in any proportion, resulting in pepper oil with high stability. Simultaneously, the method for improving the solubility of pepper oleoresin in vegetable oil using this composite solubilizer is simple and convenient. Therefore, this composite solubilizer and its method for improving the solubility of pepper oleoresin in vegetable oil have promising prospects for industrial application. Detailed Implementation

[0013] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply. Reagents or instruments whose manufacturers are not specified are all conventional products that can be purchased commercially.

[0014] Sichuan pepper oleoresin is a concentrated oily product extracted from Sichuan pepper, retaining the aroma and numbing sensation of Sichuan pepper. This product is a yellowish-brown to dark brown oily liquid that easily crystallizes at room temperature and has poor stability. To address this problem, this invention proposes a composite solubilizer comprising: linalool, sucrose isobutyrate acetate, and propylene glycol.

[0015] Sucrose isobutyrate acts as a stabilizer in the composite solubilizer of this invention, extending the stability period of Sichuan pepper oleoresin in vegetable oils. This invention, by adding sucrose isobutyrate to linalool, can extend the stability time by more than 20 times, or even longer, while simultaneously dissolving linalool.

[0016] Propylene glycol is a solubilizer for the poorly soluble fraction of pepper oleoresin in vegetable oils. Adding it can reduce the amount of precipitation after pepper oleoresin dissolves in vegetable oils.

[0017] In some embodiments, the mass percentages of linalool, sucrose isobutyrate acetate, and propylene glycol in the composite solubilizer are: linalool 24%~56%, sucrose isobutyrate acetate 17%~49%, and propylene glycol 27%~59%, which is a mass ratio of 24~56:17~49:27~59. This ratio improves the stability of the pepper oleoresin itself and its dissolution in vegetable oils, resulting in no precipitation or exudation after prolonged storage.

[0018] Preferably, the mass percentages of linalool, sucrose isobutyrate acetate, and propylene glycol in the composite solubilizer are: linalool 38%, sucrose isobutyrate acetate 24%, and propylene glycol 38%, which is a mass ratio of 38:24:38.

[0019] The composite solubilizer provided by the present invention can improve the solubility of Sichuan pepper oleoresin in vegetable oils. The Sichuan pepper oleoresin includes Sichuan pepper oleoresin obtained by supercritical carbon dioxide extraction technology. The Sichuan pepper oleoresin is prepared by a conventional supercritical carbon dioxide extraction method in the art, and the present invention does not limit this method.

[0020] Furthermore, the pepper oleoresin of the present invention can be pure oleoresin without any added ingredients, or it can be oleoresin with only added vegetable oil, or it can be oleoresin with the aromatic oil separated.

[0021] Based on the above-mentioned composite solubilizer, the present invention can also provide a pepper oil resin, which includes: the above-mentioned composite solubilizer, and pepper oil resin extracted from pepper by supercritical carbon dioxide extraction.

[0022] Sichuan pepper oleoresin is both a final product and an intermediate product. It is added to a base edible oil in a specific ratio and mixed thoroughly to prepare Sichuan pepper oil. Therefore, this invention can also provide a Sichuan pepper oil comprising the aforementioned Sichuan pepper oleoresin and vegetable oil.

[0023] In this invention, the vegetable oil used in preparing the Sichuan pepper oil is a conventional edible vegetable oil in the art, including but not limited to soybean oil, peanut oil, and rapeseed oil. This invention does not limit the choice of oil; those skilled in the art can select the appropriate oil based on the flavor objectives of the final product, the intended use, and relevant food safety standards.

[0024] Specifically, the method for improving the solubility of Sichuan pepper oleoresin in vegetable oil provided in this invention comprises the following steps: S1. The content of flavor compounds in Sichuan pepper oleoresin prepared by supercritical carbon dioxide extraction was determined by liquid chromatography.

[0025] S2. Add a composite solubilizer to the supercritical pepper oil resin to formulate pepper oil resin with standardized flavor substance content.

[0026] S3. Dissolve the pepper oleoresin obtained in S2 in vegetable oil in a certain proportion and mix well.

[0027] The flavor compounds in S1 can be substances related to numbing sensation, such as Sichuan pepper alkaloids, also known as Sichuan pepper amides, which contain numbing substances such as hydroxy-α-salicornin, hydroxy-β-salicornin, hydroxy-γ-salicornin, hydroxy-γ-isosalicornin, hydroxy-ε-salicornin, and Sichuan pepper oil.

[0028] In some embodiments, after adding the composite solubilizer in S2, the mixture is subjected to heating treatment at a temperature of 50~80℃.

[0029] Preferably, when the composite solubilizer in S2 is added to the supercritical pepper oil resin, the proportion of the composite solubilizer is ≥30%, and the pepper oil resin obtained at this proportion has higher stability.

[0030] In practical applications, those skilled in the art can adjust the formulation according to market demand. Since the standard product specification of supercritical zanthoxylum oleoresin on the market is 120 mg / g, the composite solubilizer is mostly added to this specification during experimental verification; however, this does not mean that the composite solubilizer of this invention can only be formulated to the specification of 120 mg / g. Those skilled in the art can adjust it according to other needs. Therefore, this invention does not limit the amount of composite solubilizer added.

[0031] Verification has shown that the Sichuan pepper oleoresin in S3 is miscible with vegetable oil in any proportion, and the mixture remains stable without precipitation. Therefore, the ratio of Sichuan pepper oleoresin to vegetable oil can be adjusted as needed, and this invention does not limit this adjustment.

[0032] Using the above method, pepper oil resin that is easily soluble in vegetable oil and stable over a long period of time can be obtained. This method is simple to operate, has low processing costs, makes full use of materials, and the obtained pepper oil resin remains stable after being diluted with vegetable oil, which simplifies the downstream production process and makes it convenient for food processing enterprises to use.

[0033] The features and performance of the present invention will be further described in detail below with reference to embodiments.

[0034] Example 1 This embodiment describes a composite solubilizer and the pepper oil prepared therefrom, wherein the components of the composite solubilizer are: 38% linalool, 24% sucrose isobutyrate acetate, and 38% propylene glycol.

[0035] The steps for preparing Sichuan pepper oil using the above-mentioned composite solubilizer are as follows: (1) Take 6 kg of supercritical zanthoxylum oleoresin (its ephedrine content was 200 mg / g as determined by liquid phase spectroscopy) and add it to the mixing tank.

[0036] (2) Add 4kg of compound solubilizer, heat to 60℃ and stir evenly to obtain 10kg of Sichuan pepper oil (ephedrine content 120mg / g).

[0037] (3) Take the above oleoresin and dilute it with soybean oil to concentrations of 10%, 30%, 50%, 70% and 90%, respectively. Keep the samples together with the undiluted original product for observation and leave them for 6 months.

[0038] Results: All samples were uniform and stable, with no precipitates or exudates. The diluted oil was clear and transparent with good flowability.

[0039] Example 2 This embodiment describes a composite solubilizer and the pepper oil prepared therefrom, wherein the components of the composite solubilizer are: 24% linalool, 38% sucrose isobutyrate acetate, and 38% propylene glycol.

[0040] The steps for preparing Sichuan pepper oil using the above-mentioned composite solubilizer are as follows: (1) Take 6 kg of supercritical zanthoxylum oleoresin (its ephedrine content was 200 mg / g as determined by liquid phase spectroscopy) and add it to the mixing tank.

[0041] (2) Add 4kg of compound solubilizer, heat to 60℃ and stir evenly to obtain 10kg of Sichuan pepper oil (ephedrine content 120mg / g).

[0042] (3) Take the above oleoresin and dilute it with soybean oil to concentrations of 10%, 30%, 50%, 70% and 90%, respectively. Keep the samples together with the undiluted original product for observation and leave them for 6 months.

[0043] Results: The oleoresin was viscous with slightly poor flowability. A small amount of sediment, which was a gel, appeared at the bottom of the 10% concentration diluted oil. The other samples were uniform and stable, and the diluted oil was clear and transparent.

[0044] Example 3 This embodiment describes a composite solubilizer and the pepper oil prepared therefrom, wherein the composite solubilizer comprises: 38% linalool, 17% sucrose isobutyrate acetate, and 45% propylene glycol.

[0045] The steps for preparing Sichuan pepper oil using the above-mentioned composite solubilizer are as follows: (1) Take 6 kg of supercritical zanthoxylum oleoresin (its ephedrine content was 200 mg / g as determined by liquid phase spectroscopy) and add it to the mixing tank.

[0046] (2) Add 4kg of compound solubilizer, heat to 60℃ and stir evenly to obtain 10kg of Sichuan pepper oil (ephedrine content 120mg / g).

[0047] (3) Take the above oleoresin and dilute it with soybean oil to concentrations of 10%, 30%, 50%, 70% and 90%, respectively. Keep the samples together with the undiluted original product for observation and leave them for 6 months.

[0048] Results: After 6 months of storage, the diluted oil with a concentration of less than 30% showed trace amounts of suspended matter, appearing as a mist, while the other samples were uniform and stable.

[0049] Example 4 This embodiment describes a composite solubilizer and the pepper oil prepared therefrom, wherein the composite solubilizer comprises: 49% linalool, 24% sucrose isobutyrate acetate, and 27% propylene glycol.

[0050] The steps for preparing Sichuan pepper oil using the above-mentioned composite solubilizer are as follows: (1) Take 6 kg of supercritical zanthoxylum oleoresin (its ephedrine content was 200 mg / g as determined by liquid phase spectroscopy) and add it to the mixing tank.

[0051] (2) Add 4kg of compound solubilizer, heat to 60℃ and stir evenly to obtain 10kg of Sichuan pepper oil (ephedrine content 120mg / g).

[0052] (3) Take the above oleoresin and dilute it with soybean oil to concentrations of 10%, 30%, 50%, 70% and 90%, respectively. Keep the samples together with the undiluted original product for observation and leave them for 6 months.

[0053] Results: All samples were uniform and stable, with no precipitates or exudates. The diluted oil had slightly poor light transmittance but good fluidity.

[0054] Example 5 This embodiment describes a composite solubilizer and the pepper oil prepared therefrom, wherein the components of the composite solubilizer are: 38% linalool, 24% sucrose isobutyrate acetate, and 38% propylene glycol.

[0055] The steps for preparing Sichuan pepper oil using the above-mentioned composite solubilizer are as follows: (1) Take 7 kg of supercritical zanthoxylum oleoresin (its ephedrine content was 200 mg / g as determined by liquid phase spectroscopy) and add it to the mixing tank.

[0056] (2) Add 3kg of compound solubilizer, heat to 60℃ and stir evenly to obtain 10kg of Sichuan pepper oil (ephedrine content 140mg / g).

[0057] (3) Take the above oleoresin and dilute it with soybean oil to concentrations of 10%, 30%, 50%, 70% and 90%, respectively. Keep the samples together with the undiluted original product for observation and leave them for 6 months.

[0058] Results: All samples were uniform and stable, with no precipitates or exudates. The diluted oil was slightly turbid in terms of light transmittance and had good fluidity.

[0059] Example 6 The difference from Example 1 is that the diluent used is rapeseed oil.

[0060] Results: All samples were uniform and stable, with no precipitates or exudates. The diluted oil was clear and transparent with good flowability.

[0061] Example 7 The difference from Example 1 is that peanut oil was used as the diluent.

[0062] Results: All samples were uniform and stable, with no precipitates or exudates. The diluted oil was clear and transparent with good flowability.

[0063] Example 8 The difference from Example 1 is that the diluent used is sesame oil.

[0064] Results: All samples were uniform and stable, with no precipitates or exudates. The diluted oil was clear and transparent with good flowability.

[0065] Example 9 The difference from Example 1 is that the diluent used is corn oil.

[0066] Results: All samples were uniform and stable, with no precipitates or exudates. The diluted oil was clear and transparent with good flowability.

[0067] Comparative Example 1 The difference from Example 5 is that the composite solubilizer consists of 20% linalool, 38% sucrose isobutyrate acetate, and 42% propylene glycol.

[0068] The results showed that when pepper oleoresin was added to soybean oil, a small amount of gelatinous precipitate would be formed at the bottom within 24 hours.

[0069] Comparative Example 2 The difference from Example 5 is that the composite solubilizer consists of 38% linalool, 13% sucrose isobutyrate acetate, and 49% propylene glycol.

[0070] The results showed that the pepper oleoresin sample separated into layers after 7 days of storage.

[0071] Comparative Example 3 The difference from Example 5 is that the composite solubilizer consists of 38% linalool, 38% sucrose isobutyrate acetate, and 24% propylene glycol.

[0072] The results showed that when pepper oleoresin was added to soybean oil, the mixture became cloudy and opaque, and a small amount of gelatinous precipitate would be released at the bottom within 24 hours.

[0073] Comparative Example 4 The difference from Example 1 is that the ratio of compound solubilizer to pepper oleoresin is different. Specifically, it is 2 kg of compound solubilizer and 8 kg of supercritical pepper oleoresin (the content of ephedrine was 200 mg / g as determined by liquid chromatography).

[0074] The results showed that when pepper oil resin was added to soybean oil, a gelatinous precipitate would form at the bottom within 24 hours; after 72 hours, the pepper oil resin itself would show gelatinous precipitate and naringin crystals at the bottom and on the bottle wall.

[0075] Comparative Example 5 The difference from Example 1 is that only linalool is used as the solubilizer.

[0076] Results: After 30 days of storage, crystalline precipitates appeared inside the pepper oleoresin; after adding soybean oil, the pepper oleoresin became cloudy, and a gelatinous precipitate accumulated at the bottom after 20 minutes.

[0077] Comparative Example 6 The difference from Example 1 is that only sucrose isobutyrate acetate is used as the solubilizer.

[0078] Results: The addition of Sichuan pepper oleoresin to soybean oil caused turbidity, and a gelatinous precipitate formed at the bottom within 72 hours; Sichuan pepper oleoresin itself was viscous.

[0079] Comparative Example 7 The difference from Example 1 is that only propylene glycol is used as the solubilizer.

[0080] Result: The oleoresin in Sichuan pepper oleoresin separated into layers.

[0081] Comparative Example 8 The difference from Example 1 is that linalool is replaced with limonene in the components of the composite solubilizer.

[0082] Results: After 48 hours of natural standing, crystalline precipitate appeared at the bottom of the pepper oil resin. After adding soybean oil, a gelatinous precipitate was formed at the bottom within 72 hours.

[0083] Comparative Example 9 The difference from Example 1 is that the sucrose isobutyrate ester in the composite solubilizer is replaced with mono- and diglyceride fatty acid esters.

[0084] Result: The oleoresin in Sichuan pepper oleoresin separated into layers.

[0085] Comparative Example 10 The difference from Example 1 is that propylene glycol in the composite solubilizer is replaced with medium-chain triglycerides (ODO).

[0086] Results: Pepper oleoresin precipitated as a gelatinous precipitate at the bottom within 48 hours after the addition of soybean oil.

[0087] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A composite solubilizer, characterized in that, include: Linalool, sucrose isobutyrate acetate, and propylene glycol.

2. The composite solubilizer according to claim 1, characterized in that, The mass ratio of linalool, sucrose isobutyrate acetate to propylene glycol in the composite solubilizer is 24~56:17~49:27~59.

3. The composite solubilizer according to claim 2, characterized in that, The mass ratio of linalool, sucrose isobutyrate acetate, and propylene glycol in the composite solubilizer is 38:24:

38.

4. The use of the composite solubilizer according to any one of claims 1 to 3 in the preparation of products for improving the solubility of pepper oleoresin in vegetable oils.

5. The application according to claim 4, characterized in that, The pepper oil resin was obtained by supercritical carbon dioxide extraction.

6. The application according to claim 5, characterized in that, The pepper oleoresin includes pure oleoresin, oleoresin with added vegetable oil, or oleoresin from which aromatic oils have been separated.

7. A pepper oil resin, characterized in that, include: The composite solubilizer according to any one of claims 1 to 3, and the pepper oleoresin extracted from pepper by supercritical carbon dioxide extraction.

8. A kind of Sichuan pepper oil, characterized in that, It includes the pepper oleoresin and vegetable oil as described in claim 7.

9. A method for improving the solubility of Sichuan pepper oleoresin in vegetable oil, characterized in that, include: The composite solubilizer according to any one of claims 1 to 3 is added to the pepper oil resin prepared by supercritical carbon dioxide extraction, mixed well, and then diluted with vegetable oil to the target concentration.

10. The method according to claim 9, characterized in that, The composite solubilizer is heated when mixed with pepper oil resin at a temperature of 50-80°C.