Butter-flavor solid zanthoxylum oil

Abstract

The invention relates to the technical field of edible seasoning oil preparation, and particularly discloses beef tallow-flavored solid zanthoxylum oil which comprises 14.0-20.0% of seasonal zanthoxylum, 0-0.8% of zanthoxylum volatile essence, 0-0.05% of rosemary extract and the balance of refined beef tallow. According to the invention, the beef tallow base provides rich fat phase taste and enhances the fat-soluble fragrance carrier effect; a staged extraction strategy is matched, so that the numb feeling and the aroma are coordinated in strength and release time sequence, the overall acceptance is improved, and available flavor substances in an oil phase can be recovered to the maximum extent through staged extraction and ultrahigh recovery procedures; the residues are subjected to secondary extraction or drying and crushing for feed and organic fertilizer, so that the value of the raw materials can be maximized, the waste treatment cost is reduced, and a process closed loop is formed.

Description

Technical Field

[0001] This invention belongs to the field of edible seasoning oil preparation technology, specifically relating to a butter-flavored solid Sichuan pepper oil. Background Technology

[0002] Sichuan peppercorns, a traditional Chinese spice, are used to make Sichuan peppercorn oil, which is widely used in Sichuan cuisine and various catering and food processing settings due to its unique fragrant and numbing flavor. Currently, the main production processes for Sichuan peppercorn oil on the market include traditional frying, oil immersion, supercritical CO2 extraction, and solvent extraction. However, existing technologies still have many shortcomings in terms of product taste, flavor harmony, production stability, and raw material utilization, making it difficult to meet consumers' demand for high-quality compound seasoning oil.

[0003] Existing Sichuan pepper oils mostly use single vegetable oils (such as rapeseed oil and soybean oil) as carriers, lacking optimized design for the lipid phase's ability to carry flavor and aroma. The low density of single vegetable oil phases limits their ability to carry lipid-soluble aroma substances (such as terpenes, aromatic aldehydes, and ketones) in Sichuan pepper, resulting in a thin flavor and a short-lasting release of the numbing and aromatic flavor. Some processes have attempted to use compound oils, but without a scientifically sound ratio. Either the oils are too fluid, causing the aroma to evaporate too quickly, or the viscosity is too high, affecting ease of use. Furthermore, the synergistic effect of different oils on the dissolution of Sichuan pepper flavor substances has not been considered.

[0004] In response, this application proposes a butter-flavored solid Sichuan pepper oil to solve the above problems. Summary of the Invention

[0005] The purpose of this invention is to provide a butter-flavored solid Sichuan pepper oil to solve the problems mentioned in the background art.

[0006] To achieve the above objectives, the present invention provides the following technical solution:

[0007] A butter-flavored solid Sichuan peppercorn oil, comprising:

[0008] Seasonal Sichuan pepper 14.0%–20.0%, Sichuan pepper volatile essence 0%–0.8%, rosemary extract 0–0.05%, the remainder being refined butter.

[0009] A butter-flavored solid Sichuan peppercorn oil, comprising the Sichuan peppercorn oil as described above, wherein the method includes the following steps:

[0010] S1. Low-temperature cold crushing: Cleaned seasonal peppercorns are cold crushed at low temperature to a particle size of 0.5–2.0 mm to obtain broken seasonal peppercorn fragments.

[0011] S2. Low-temperature soaking: Heat the refined butter to 80-95°C and turn off the heat. Then add 70% to 80% of the total amount of the broken seasonal peppercorns to the refined butter and soak for 30 minutes using the residual heat to obtain the preliminary soaking oil.

[0012] S3. Heating extraction: The initial impregnation oil is heated to 100–110°C and maintained for 20–30 minutes until the peppercorns turn dark and the bubbles in the pot are significantly reduced, in order to enhance the fat-soluble flavor and pigment dissolution, and obtain a rich aroma intermediate oil.

[0013] S4. High-temperature aroma stimulation: Raise the oil temperature to 120-130℃, add the remaining broken seasonal peppercorns and peppercorn volatile essence, stimulate the aroma for 30-60 seconds, then immediately turn off the heat to obtain the aroma-stimulating oil.

[0014] S5. Constant temperature esterification: Remove the butter from the heat and cool it to 50-60℃ for 6-12 hours for constant temperature esterification.

[0015] S6. Ultra-high pressure pressing: The oil is pressed using an ultra-high pressure oil press to obtain pressed oil.

[0016] S7. Filtering and packaging: After the pressed oil is naturally cooled to room temperature, it is filtered through a filter screen, and the rosehip extract is added and mixed well. The mixture is then sealed and stored to obtain solid butter-flavored Sichuan pepper oil.

[0017] Preferably, in step S1, the low-temperature cold crushing is carried out by mechanical rolling or shearing to achieve a cell wall breakage rate of ≥65%, and the particle size of the dried crushed material is controlled within 0.5–1.5 mm.

[0018] Preferably, the slow heating rate in step S3 is 2–4 °C / min, and the temperature is raised to 105 ± 3 °C and held for 25 ± 5 minutes.

[0019] Preferably, the high-temperature aroma stimulation in step S4 is performed by two intermittent heatings, each lasting 30–45 seconds, with a cooling period of 1–3 minutes between heatings to prevent overheating and decomposition of the oils.

[0020] Preferably, the rosemary extract is added at a mass ratio of 0.01% to 0.03% of the pressed oil.

[0021] Compared with the prior art, the beneficial effects of the present invention are:

[0022] (1) In this invention, the butter base provides a rich lipid phase taste and enhances the effect of lipid-soluble aroma carrier; combined with the staged extraction strategy, the numbing sensation (alkylamides) and aroma (terpenes, aromatic aldehydes and ketones, etc.) are coordinated in terms of intensity and release sequence, improving the overall acceptability; the segmented extraction and ultra-high recovery (or centrifugation / pressing) process can maximize the recovery of usable flavor substances in the oil phase; the secondary extraction or drying and pulverization of the residue for use in feed and organic fertilizer can maximize the value of raw materials and reduce waste treatment costs, forming a closed-loop process.

[0023] (2) In this invention, parameters such as segmented temperature control, quantitative soaking time and cell wall breaking particle size reduce the impact of raw material and process fluctuations on the final flavor; combined with a staged extraction strategy, the numbing sensation (alkylamides) and aroma (terpenes, aromatic aldehydes and ketones, etc.) are coordinated in terms of intensity and release sequence, thereby improving overall acceptability. Attached Figure Description

[0024] Figure 1 This is a flowchart of a butter-flavored solid Sichuan pepper oil according to the present invention. Detailed Implementation

[0025] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0026] Example 1:

[0027] Please see Figure 1 As shown, a butter-flavored solid Sichuan peppercorn oil comprises:

[0028] Raw material description: The seasonal peppercorns are cell wall broken pieces that are dried at low temperature after harvesting and then cold-crushed and sieved (see step S1); the beef tallow is pre-refined edible beef tallow.

[0029] Experimental replication: Three parallel samples (n=3) were prepared and measured independently for each example / control, and the results were taken as arithmetic mean ± standard deviation.

[0030] Overview of data acquisition / analysis methods:

[0031] Numbing active ingredient (quantified by the main alkyl amide "sanshool"): HPLC-UV quantification, C18 column, mobile phase acetonitrile: water gradient, detection wavelength 254nm, external standard method quantification, sample pretreatment was methanol ultrasonic extraction followed by centrifugation and filtration (0.22μm).

[0032] Total volatile aroma (sum of several key terpenes and aromatic substances): SPME-GC-MS (DB-5 capillary column), internal standard method (tributyl phthalate or known internal standard), the total peak area was obtained by identification by target ion / retention time and integration and converted to mg / kg.

[0033] Sensory evaluation: A trained sensory group of 10 people evaluated the sensory aspects using a 0–10 scale (aroma intensity, numbing sensation intensity, overall acceptability), with the average score for each aspect ± SD.

[0034] Peroxide value (PV) and acid value (AV): determined by titration method specified by AOAC / national standard, with units of meq O2 / kg and mg KOH / g, respectively.

[0035] Color (L*a*b* or Lovibond): The L* value is measured using a portable colorimeter (the larger the value, the lighter the color).

[0036] Statistical analysis: One-way ANOVA was performed on the three groups of data. A p < 0.05 was used to determine that the difference was significant (marked with "*" when indicating significance in the table).

[0037] Specifically, the multiple solutions consist of the following:

[0038] Option 1:

[0039] formula:

[0040] Refined beef tallow: 8.50 kg;

[0041] Seasonal Sichuan peppercorns (low-temperature cold-crushed material): 2.0 kg;

[0042] Sichuan pepper volatile essence (optional aroma enhancement): 0.05kg;

[0043] Rosemary extract: 3.0g;

[0044] Preparation steps:

[0045] The process of breaking down and conditioning Sichuan peppercorns involves cold-breaking 0.80 kg of cleaned seasonal Sichuan peppercorns at low temperature to an average particle size of 0.8 mm, resulting in broken-down seasonal Sichuan peppercorn fragments.

[0046] Operating details: Process with a cold crusher (roller shear) for 3 minutes, and sieve to a size of 0.5–1.5 mm; dry in a drying oven at 45°C with moderate airflow until the moisture content is below 6%.

[0047] Low-temperature maceration extraction: 2.0 kg of crushed seasonal peppercorns was added to preheated purified butter and kept at a constant temperature of 85°C with slow stirring for 40 minutes to obtain the initial maceration oil.

[0048] Proportion Explanation: The ratio of seasonal peppercorn fragments to the final oil mass during cell wall breaking is 8.0%. The operation is completed in a sealed reactor to reduce volatilization loss.

[0049] Slowly increasing the temperature enhances extraction. The initial impregnation oil is heated to 105°C at a rate of 3°C / min and held for 25 minutes to enhance the dissolution of fat-soluble flavors and pigments, resulting in a rich and aromatic intermediate oil.

[0050] Process control: Stir continuously and slowly during the heating process and monitor the temperature curve.

[0051] Short-term high-temperature aroma stimulation involves intermittently heating the rich aroma intermediate oil to 125°C twice (40 seconds each time, with a 2-minute interval), adding the volatile essence of Sichuan pepper to trigger the release of secondary aromas and quickly terminate the reaction, resulting in an aroma-stimulating oil.

[0052] Objective: To release and fix secondary aromas with short bursts of aroma to prevent prolonged thermal decomposition of oils.

[0053] The mixture is finely filtered and formulated with antioxidants and then filled. After cooling the aromatic oil to 55±2℃, it is finely filtered through 1.0μm, and rosemary extract (3.0g) is added at 42℃ and stirred evenly. Finally, it is filled, sealed and cooled in a low-microbial filling workshop to obtain the final product, butter-flavored solid Sichuan pepper oil.

[0054] Quality control point: Samples are taken from the outlet for PV, AV, HPLC, GC-MS and sensory testing.

[0055] As can be seen from the above, the segmented extraction and ultra-high recovery (or centrifugation / pressing) process can maximize the recovery of usable flavor substances in the oil phase; the secondary extraction or drying and pulverization of the residue for use in feed and organic fertilizer can maximize the value of raw materials and reduce waste treatment costs, forming a closed-loop process.

[0056] Option 2:

[0057] Refined butter: 7.00 kg;

[0058] Seasonal Sichuan peppercorns (low-temperature cold-crushed material): 1.60 kg;

[0059] Sichuan pepper volatile essence: 0.08kg;

[0060] Rosemary extract: 2.0g;

[0061] Preparation steps:

[0062] The process involves breaking down and conditioning Sichuan peppercorns. 0.60 kg of cleaned seasonal Sichuan peppercorns are cold-crushed at low temperature until the average particle size is 0.9 mm, resulting in broken seasonal Sichuan peppercorn fragments.

[0063] Low-temperature maceration extraction involves adding crushed seasonal Sichuan peppercorns (6.0%) to preheated purified butter, maintaining the temperature at 88°C, and stirring slowly for 50 minutes to obtain the initial maceration oil.

[0064] Extraction was enhanced by slow heating. The initial impregnation oil was heated to 108°C at a rate of 3°C / min and held for 20 minutes to enhance the dissolution of volatile and fat-soluble substances, thus obtaining an intermediate oil.

[0065] Short-term high-temperature aroma stimulation is used to briefly heat the intermediate oil to 128°C (45 seconds), add the volatile essence of Sichuan pepper to stimulate the aroma, and obtain an aroma-stimulating oil.

[0066] The oil is finely filtered and formulated with antioxidants and then filled. The oil is cooled to 50–55°C, finely filtered through 1.0 μm, and then rosemary extract (2.0 g) is added at 42°C and stirred before filling to obtain the finished butter-flavored solid Sichuan pepper oil.

[0067] In contrast, the traditional method is as follows:

[0068] Refined butter: 8.00 kg;

[0069] Seasonal Sichuan peppercorns: 1.50 kg;

[0070] Traditional preparation (single-step high-temperature long-time impregnation):

[0071] 0.50 kg of seasonal Sichuan peppercorns are directly added to 8.00 kg of hot oil and heated to 130°C for 60 minutes to obtain a high-temperature immersion oil (traditional immersion oil).

[0072] After cooling, the product undergoes simple filtration and is filled at room temperature to obtain the finished product.

[0073] Note: The control group used traditional high-temperature long-term immersion.

[0074] V. Test Items, Measurement Methods, and Results;

[0075] Sampling and Sample Processing:

[0076] After each batch is completed, a sample (100g) is taken at the outlet and divided into 3 parallel samples (different parallel batches) for HPLC, GC-MS, PV / AV, color and sensory testing, respectively.

[0077] HPLC: The sample was extracted with methanol (HPLC grade) by ultrasonication for 30 min, centrifuged for 10 min (10000 rpm), and the supernatant was filtered through a 0.22 μm filter before injection. Pure Sanshool standard was used as the external standard. The linear range was 0.1–100 mg / L, R0. 2 >0.999.

[0078] GC-MS (SPME): 2g of sample was placed in a 20mL glass bottle, internal standard was added, equilibrated at 40℃, SPME sampling was performed for 30min, and then GC-MS analysis was performed. The target compound was confirmed by comparison with the mass spectral library according to the retention time and quantified using the internal standard.

[0079] Sensory panel: 10 trained reviewers (blind testing), each independently scored the blind sample (0–10 points), and rated the aroma, tingling sensation, and overall acceptability. Scores were averaged ± SD.

[0080] PV / AV: Determined by titration according to national standard method, with the average value taken from three replicates.

[0081] Results (all mean ± standard deviation, n = 3; sensory evaluation is the mean ± SD of 10 people's ratings).

[0082] Table 1 below shows the comprehensive comparison data of the three groups (Scheme 1, Scheme 2, and Control).

[0083] Table 1

[0084]

[0085]

[0086] Definition and calculation method of effective component recovery rate of Sichuan pepper: Based on the total sanshool mass (mg) measured in the pre-treatment of the Sichuan pepper added at the time of application, the recovery rate = (total sanshool detected in the final oil (mg) ÷ total sanshool in the original Sichuan pepper (mg)) × 100%.

[0087] Before preparation, a representative sample of each batch of Sichuan pepper was taken and quantified by HPLC to calculate the original content.

[0088] As shown in the table above, the recovery rate of active ingredients and the intensity of tingling sensation were significantly improved (Scheme 1 > Scheme 2 > Control).

[0089] Scheme 1 employs a segmented temperature control strategy of first low-temperature immersion, then slow heating, and finally short-term aroma stimulation. Combined with sufficient cell wall disruption (0.8 mm particle size, high cell wall disruption rate) and a moderate immersion time (40 min), it facilitates efficient and gentle extraction of alkylamides (such as sanshool). HPLC quantitative results show that Scheme 1 yielded 42.0 mg / kg of sanshool with a recovery rate of 78%, which is approximately 33 percentage points higher than the traditional control recovery rate (from 45% to 78%). The corresponding sensory numbing sensation score increased from 4.6 to 7.6, meeting the technical objective of "balancing flavor and functionality".

[0090] Retention of volatile aromas and enhancement of aroma intensity:

[0091] GC-MS total volatile matter content showed that Scheme 1 was 560 mg / kg, which was much higher than the control's 340 mg / kg. This indicates that segmented temperature control (low temperature to first dissolve light volatile components, slow temperature increase to extract mid-to-late aromas, and then short-term aroma stimulation to trigger secondary aromas) can better preserve and release aroma molecules with different boiling point ranges, thus the aroma intensity is significantly better than the control in sensory tests.

[0092] Inhibits oxidative degradation and improves stability (lower PV and AV):

[0093] The PV of Scheme 1 was 1.8 meq O2 / kg (compared to 3.5), and the AV was 0.12 mg KOH / g (compared to 0.30). This indicates that the process of fine filtration plus the addition of natural antioxidants at a lower temperature effectively reduced thermal oxidation and the generation of trace free fatty acids, thereby improving the initial stability and shelf life potential of the finished product.

[0094] Sensory experience and acceptance:

[0095] The overall sensory results showed that the overall acceptance of Scheme 1 was 8.6 (excellent), Scheme 2 was 8.1 (good), and the control was only 6.2. This indicates that the process of the present invention not only improved the index data, but also achieved a higher consumer experience (harmony of taste / aroma / numbing sensation).

[0096] Comparison between examples (process adjustability):

[0097] Option 2 is used to achieve a richer surface aroma (with still high sensory aroma fraction), but it has a slightly lower sanshool recovery rate than Option 1 (38.2 vs 42.0 mg / kg).

[0098] As can be seen from the above, low-temperature cold breaking destroys the cell wall and oil cell structure of Sichuan pepper, significantly increasing the solid-oil phase contact interface; the subsequent lipid phase impregnation makes it easier for lipid-soluble or semi-lipid-soluble active ingredients such as alkyl amides and volatile terpenes to migrate into the oil phase, thereby improving the release and dissolution efficiency of active flavor components.

[0099] By employing a segmented temperature control strategy of "low temperature and gentle dissolution → slow temperature increase to extract mid and late notes → short-term high temperature to stimulate aroma", the aroma components can be extracted and retained in batches according to volatility and thermal stability, thereby forming a multi-layered aroma structure of top, middle and base notes in the final product, avoiding the loss of light volatile components or high temperature degradation caused by one-time high temperature.

[0100] Replacing prolonged high-temperature treatment with short-duration, high-intensity, but intermittent "flash" can trigger the desired secondary aroma release while minimizing heat exposure time, thereby reducing fat oxidation byproducts and burnt flavor, and improving the purity of taste;

[0101] At lower temperatures, the combination of natural antioxidants (rosemary extract) can inhibit the initiation and propagation of free radical chain reactions, thereby reducing the formation rate of peroxides and free acids and improving the initial oxidation stability of the product. Fine filtration can remove trace amounts of irritating low-boiling substances (such as certain aldehydes and secondary amines), while the control of short-term aroma stimulation can avoid the excessive release of sharp, highly volatile irritating components, resulting in a more rounded aroma and a more moderate numbing sensation in the final product.

[0102] The butter base provides a rich, oily mouthfeel and enhances the effect of fat-soluble aroma carriers; combined with a staged extraction strategy, the numbing sensation (alkylamides) and aroma (terpenes, aromatic aldehydes and ketones, etc.) are coordinated in terms of intensity and release sequence, improving overall acceptability;

[0103] Using plant-based rosemary extract as an antioxidant system can reduce reliance on synthetic antioxidants and make it easier to highlight the advantages of "natural antioxidants / no synthetic additives" on the label, which aligns with current consumer preferences for natural and healthy foods.

[0104] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A butter-flavored solid Sichuan peppercorn oil, characterized in that, The Sichuan pepper oil comprises, by weight percentage: Seasonal Sichuan pepper 14.0%–20.0%, Sichuan pepper volatile essence 0%–0.8%, rosemary extract 0–0.05%, the remainder being refined butter.

2. The butter-flavored solid Sichuan peppercorn oil according to claim 1, characterized in that, The method for preparing Sichuan pepper oil includes the following steps: S1. Low-temperature cold crushing: Cleaned seasonal peppercorns are cold crushed at low temperature to a particle size of 0.5–2.0 mm to obtain broken seasonal peppercorn fragments. S2. Low-temperature soaking: Heat the refined butter to 80-95°C and turn off the heat. Then add 70% to 80% of the total amount of the broken seasonal peppercorns to the refined butter and soak for 30 minutes using the residual heat to obtain the preliminary soaking oil. S3. Heating extraction: The initial impregnation oil is heated to 100–110°C and maintained for 20–30 minutes until the peppercorns turn dark and the bubbles in the pot are significantly reduced, in order to enhance the fat-soluble flavor and pigment dissolution, and obtain a rich aroma intermediate oil. S4. High-temperature aroma stimulation: Raise the rich aroma intermediate oil to 120-130℃, add the remaining broken seasonal peppercorn fragments and peppercorn volatile essence, stimulate aroma for 30-60 seconds and then turn off the heat to obtain the aroma-stimulating oil. S5. Constant temperature esterification: Remove the aromatic oil from the heat and cool it to 50-60℃ for constant temperature esterification for 6-12 hours to obtain the oil. S6. Ultra-high pressure pressing: The oil is pressed using an ultra-high pressure oil press to obtain pressed oil; S7. Filtering and packaging: After the pressed oil is naturally cooled to room temperature, it is filtered through a filter screen, and the rosehip extract is added and mixed well. The mixture is then sealed and stored to obtain solid butter-flavored Sichuan pepper oil.

3. The butter-flavored solid Sichuan pepper oil according to claim 2, characterized in that, In step S1, the low-temperature cold crushing is carried out by mechanical rolling or shearing to achieve a cell wall breakage rate of ≥65%, and the particle size of the dried crushed material is controlled within 0.5–1.5 mm.

4. The butter-flavored solid Sichuan peppercorn oil according to claim 2, characterized in that, The slow heating rate in step S3 is 2–4 °C / min, and the temperature is raised to 105 ± 3 °C and held for 25 ± 5 minutes.

5. The butter-flavored solid Sichuan peppercorn oil according to claim 2, characterized in that, The high-temperature aroma stimulation in step S4 is performed by two intermittent heating sessions, each lasting 30–45 seconds, with a cooling period of 1–3 minutes between heating sessions to prevent the oils from overheating and decomposing.

6. The butter-flavored solid Sichuan peppercorn oil according to claim 2, characterized in that, The rosemary extract is added at a mass ratio of 0.01%–0.03% of the pressed oil.

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