Patent Document: Separation Method to Enhance the Flavor and Unsaturated Fatty Acid Content of Butter Fat (Beef Tallow)

Patent Number: CN121873880A
Publication Date: February 9, 2026
Application Number: CN202610183575.4A
Current Status: Pending
Assignee: Shanghai Institute of Technology (上海应用技术大学)
Inventors: The inventors are not specifically named in this excerpt; the patent would typically list individual researchers affiliated with Shanghai Institute of Technology.

Technical Field

The present invention relates to the technical field of food processing, and specifically to a separation method for improving beef tallow (butter fat) flavor and unsaturated fatty acid content.

Background of the Invention

Edible beef tallow is processed and refined from fresh, clean, and intact beef fat. It appears white or light yellow, has a fine and smooth taste with mellow flavor, and is rich in nutrients such as fatty acids, vitamins, and minerals. Beef tallow possesses excellent thermal stability and oxidation stability, along with fine texture characteristics and mellow flavor properties, making it widely applied in food processing fields including shortening, margarine, edible essences, and hotpot condiments.

However, beef tallow contains high levels of highly Saturated Fatty Acids (SFA) such as stearic acid and palmitic acid. Long-term consumption of these saturated fats can lead to hypertension, hyperlipidemia, and cardiovascular disease. Furthermore, the high melting point of beef tallow presents certain limitations in some food processing applications.

Therefore, the development of beef tallow products with:

• Low Saturated Fatty Acid (SFA) content
• High flavor complexity
• Excellent storage stability

has become a research hotspot in the field of high-value utilization of livestock byproducts. Such products have potential applications as functional fats in food processing, including baking shortenings and margarines.

Current Fractionation Techniques and Their Limitations

Currently, fractionation is commonly used to reduce the saturation of fats and oils. Common oil fractionation methods include:

Therefore, the development of a beef tallow separation method capable of achieving dual optimization of nutrition and flavor has great practical significance.

Summary of the Invention

Technical Problem

Due to the defects in the prior art, the present invention provides a beef tallow separation method capable of achieving dual optimization of nutrition and flavor.

Technical Solution

The present invention specifically relates to a separation method for improving beef tallow flavor and unsaturated fatty acid content, which utilizes molecular distillation in a sectionalized manner to achieve:

• Cooperative optimization of highly unsaturated fatty acid enrichment
• Directional improvement of fat flavor

Short-Path Molecular Distillation Technology Advantages:

• Low distillation pressure
• Low operation temperature
• Short heating time
• High separation efficiency
• Particularly suitable for separating oils/fats or other heat-sensitive substances and bioactive compounds

Key Benefits of This Technology:

• Reduces loss of heat-sensitive nutrient components
• Avoids loss of flavor substances caused by pyrolysis or excessive volatilization
• Enables directional enrichment of flavor substances through temperature gradient design
• Simple operation, suitable for processing different foods
• No introduction of other chemical substances or thermal decomposition
• Products show wide melting point range and different fatty acid contents
• Demonstrates different melting point characteristics for different beef tallow fractions
• Balances nutrition and flavor considerations
• Widely applicable to food fields such as baking and hotpot condiments

Basic Method Steps

A separation method for improving the flavor and unsaturated fatty acid content of beef tallow comprises:

1. Balancing: Refined beef tallow is equilibrated at room temperature
2. Heating: The beef tallow is heated in a water bath until completely transparent and liquid
3. Molecular Distillation: Short-path molecular distillation is performed on the completely transparent liquid beef tallow to obtain separated beef tallow

Distillation Temperature Range: 160–210°C

• Too low temperature results in lower yields
• Too high temperature results in loss of nutrients and heat-sensitive substances

Detailed Process Parameters

Preferred Technical Solutions

Balancing Conditions:

• Equilibration time: Not less than 30 minutes
• Water bath temperature: 50–55°C (to achieve clear liquid state)

Short-Path Molecular Distillation Conditions:

• Equipment: Short-path molecular distillation instrument
• Vacuum degree in distillation chamber: Lower than 0.1 MPa
• Chilled water circulation: Started
• Light phase component condensation temperature: 50–55°C
• Feeding rate: 50–55 drops/min
• Film scraping rotating speed: 200–250 r/min

Preferred Distillation Temperature: 160–180°C

Product Characteristics

Unsaturated Fatty Acid Content

• Mass ratio of unsaturated fatty acids in separated beef tallow: ≥ 55%
• Improvement: Increases from 40.85 g/100g (raw material) to 57 g/100g

Flavor Enhancement

• Fat flavor characteristic substances (such as trans,trans-2,4-decadienal and E-2-octenal):
  • Content improved by at least 1.5 times (2–3 times) compared to refined beef tallow
  • Confirmed through GC-MS detection
• Sensory evaluation:
  • Descriptive sensory analysis shows fat flavor organoleptic evaluation score improved by at least 40% compared to refined beef tallow
  • Comprehensive flavor acceptance significantly improved

Melting Point Characteristics

• Raw material melting point: 44.1°C (single melting point)
• Separated products: Stepped melting point system at 32.07–43.13°C
• Different fractions match different food processing scenarios:
  • Low melting point fractions: Seasoning oils
  • Medium melting point fractions: Baked shortbread
  • High melting point fractions: Artificial butter

Advantages and Beneficial Effects

(1) Improved Nutritional Value:

• Unsaturated fatty acid content increased from 40.85 g/100g to 57 g/100g
• Significantly enhances the nutritional profile of the product

(2) Enhanced Flavor:

• Content of characteristic fat flavor substances (trans,trans-2,4-decadienal and E-2-octenal) increased by 1.5–2.3 times
• Material basis for flavor improvement clarified through GC-MS detection
• Fat flavor intensity improved by more than 40% compared to raw materials
• Comprehensive flavor acceptance significantly improved
• Solves the problem of difficulty in achieving both nutrition and flavor in prior art

(3) Improved Suitability Through Melting Point Modification:

• Single melting point of raw material (44.1°C) converted to a stepped melting point system (32.07–43.13°C)
• Low, medium, and high melting point fractions can respectively match different food processing scenarios:
  • Seasoning oil
  • Baked shortbread
  • Artificial butter
• Breaks through the bottleneck of limited application range of traditional beef tallow
• Achieves high-value utilization with "one material, multiple uses"
• Good application prospects

Experimental and Analytical Methods

Yield Calculation

Light phase yield of beef tallow is calculated as:

Light phase yield (%) = (m₁ - m₀) / 500 × 100%

Where:

• m₁ = mass (g) of receiving bottle collecting the light phase component
• m₀ = receiving flask mass (g) for collecting the light phase

Fatty Acid Content Determination

Method: Gas chromatography-mass spectrometry, reference GB/T5009.168-2016

Procedure:

1. Saponification and Methyl Esterification:
   • Take 0.1g product, add 500 μL of 10 mg/mL methyl tridecanoate as internal standard
   • Add 8 mL of 2% sodium hydroxide methanol solution
   • Reflux on 80±1°C water bath until oil droplets disappear
2. Derivatization:
   • Add 7 mL of 15% boron trifluoride methanol solution from reflux condenser upper end
   • Continue reflux for 2 min on 80±1°C water bath
3. Cooling:
   • Rinse reflux condenser with small amount of water
   • Stop heating, remove flask from water bath, rapidly cool to room temperature
4. Extraction:
   • Accurately add 10–30 mL n-heptane, shake for 2 min
   • Add saturated sodium chloride aqueous solution, allow to stand for layering
   • Pipette about 5 mL of upper n-heptane extract
   • Add about 3–5 g anhydrous sodium sulfate to 25 mL test tube, shake for 1 min, stand for 5 min
   • Pipette 1 mL of upper layer solution into sample vial
5. Chromatographic Conditions:
   • Column: DB-5 (30 mm × 0.25 μm × 0.25 mm)
   • Injection volume: 0.1 μL
   • Constant flow rate: 1.0 mL/min
   • Split ratio: 20:1
   • Carrier gas: Helium
   • Inlet temperature: 240°C
   • Temperature program: Initial 150°C for 2 min; increase to 200°C at 15°C/min; increase to 224°C at 2°C/min; final increase to 270°C at 10°C/min, hold for 10 min

Melting Point Determination

Method: Reference GB/T12766-2008 animal fat melting point measurement

Procedure:

1. Sample Preparation:
   • Insert capillary tube into thawed sample, aspirate 1 cm ± 2 mm fat column
   • Wipe outer surface with paper towel
   • Place capillary against outer surface of beaker containing ice cubes, cool for a few seconds to solidify fat
   • Place in cooling water bath for 5 minutes
2. Assembly:
   • Fix cooled capillary containing beef tallow sample and precision thermometer together
   • Ensure fat near capillary bottom is level with mercury bulb
3. Heating Setup:
   • Pour half cup of pre-boiled and cooled water into 500 mL beaker
   • Suspend thermometer with fixed capillary in water
   • Ensure bottom of mercury bulb is 30 mm from water surface
4. Heating Protocol:
   • Regulate initial temperature of electric heating source to below expected melting point
   • Stir to ensure heating rate of 3–4°C per minute
   • When approaching melting point, reduce heating rate to 0.5°C per minute
5. Observation:
   • Continue heating until grease column in capillary begins to rise
   • Observe rising temperature - this is the melting point of the sample

Sensory Analysis

Method: Reference GB/T46555-2025 "Selection and training of sensory evaluation for sensory analysis"

Procedure:

1. Panel Training:
   • Panelists received specialized training to identify and define aroma descriptive terms
   • Finalized 6 aroma attributes to describe tallow samples:
     • Dairy aroma
     • Beef flavor
     • Fat flavor
     • Sweet taste
     • Baking flavor
     • Sweat odor
   • Scoring system: 0–5 metric scale
     • 0 = imperceptible
     • 1 = weakly perceptible
     • 2 = slightly noticeable
     • 3 = moderately noticeable
     • 4 = strongly noticeable
     • 5 = very strongly
2. Sample Preparation:
   • Melt samples in 50°C constant temperature water bath
   • Place 1.0g in numbered brown sealed bottles
   • Place in 50°C incubator tray for presentation
3. Evaluation:
   • Panelists sniff samples in random order
   • Each member repeats evaluation of all samples 3 times
   • Final score for each fragrance attribute = average score of 3 evaluations from 12 panelists

Aroma Compound Quantitative Analysis

Procedure:

1. SPME Fiber Preparation:
   • Prior to extraction, age SPME extraction heads (DVB/CAR/PDMS, 50/30 μm) for 15 min at 250°C
2. Extraction:
   • Accurately weigh 1g sample, place in 20 mL headspace bottle
   • Add 2.5 μL of 100 mg/L o-dichlorobenzene as internal standard
   • Seal with bottle cap containing septum
   • Place in heat-collection constant temperature heating magnetic stirrer
   • Stir and equilibrate for 30 min at 60°C
3. Desorption:
   • After extraction completion, insert fiber head into GC inlet
   • Desorb in splitless mode for 5 min at 250°C
4. Chromatographic Conditions:
   • Instrument: GC-MS (Agilent Technologies)
   • Column: DB-WAX capillary (30 m × 250 μm × 0.25 μm)
   • Inlet temperature: 250°C
   • Temperature program:
     • Initial: 40°C for 3 min
     • Increase to 180°C at 4°C/min, hold for 2 min
     • Increase to 250°C at 35°C/min, hold for 2 min
   • Carrier gas: High purity helium (99.999%) at 1.2 mL/min
5. Mass Spectrometry Conditions:
   • Ion source: EI at 240°C
   • Ionization voltage: 70 eV
   • Scan range: 33–450 amu
   • Identification: Computer NIST2022 mass spectrum database comparison
   • Quantification: Internal standard method

Statistical Analysis

• SPSS 27.0 software for data analysis
• Multiple comparison analysis for data comparison
• Minimum 3 replicates per experiment
• Results expressed as mean ± standard deviation

Examples

Example 1 (160°C Distillation Temperature)

Procedure:

1. Take refined beef tallow stored at 4°C, equilibrate at room temperature for 30 min
2. Accurately weigh 500g beef tallow using electronic analytical balance, transfer to pre-dried 500 mL glass beaker
3. Place beaker containing refined beef tallow into constant-temperature water bath at 55°C until completely transparent
4. Start short-path molecular distillation instrument, set distillation temperature to 160°C
5. Start vacuum pump, stably control vacuum degree in distillation chamber to 0.1 MPa
6. Start chilled water circulation, set light phase component condensation temperature to 50°C
7. After instrument parameters stabilize, slowly pour beef tallow into feed inlet
   • Feed rate: 50 drops/min
   • Scraping rotation speed: 200 r/min
8. Obtain separated beef tallow

Example 2 (170°C Distillation Temperature)

Same as Example 1, except distillation temperature is 170°C.

Example 3 (180°C Distillation Temperature)

Same as Example 1, except distillation temperature is 180°C.

Example 4 (190°C Distillation Temperature)

Same as Example 1, except distillation temperature is 190°C.

Example 5 (200°C Distillation Temperature)

Same as Example 1, except distillation temperature is 200°C.

Example 6 (210°C Distillation Temperature)

Same as Example 1, except distillation temperature is 210°C.

Experimental Results

Light Phase Yield (Figure 1)

Unsaturated Fatty Acid Content (Figure 5)

Melting Points (Figure 2)

Fat Flavor Sensory Scores (Figure 3)

Key Finding: Fat flavor organoleptic evaluation score improved by at least 40% compared to refined beef tallow.

Aroma Compounds Enhancement (Figure 4)

• Content of fat flavor characteristic substances (trans,trans-2,4-decadienal and E-2-octenal) in separated beef tallow:
• Increased by 2–3 times compared to refined beef tallow
• Confirmed through GC-MS detection

Drawings

The patent includes the following figures:

• FIG. 1: Comparative schematic diagram of the yields from Examples 1–6
• FIG. 2: Schematic diagram showing the sliding melting point comparison of refined tallow (without molecular distillation treatment) and separated tallow obtained in Examples 1–6
• FIG. 3: Sensory radar contrast diagram of refined tallow (without molecular distillation treatment) and separated tallow obtained in Examples 1–6
• FIG. 4: Comparison graph of aroma compound profiles of refined tallow (without molecular distillation treatment) and separated tallow obtained in Examples 1–6
• FIG. 5: Graph showing fatty acid composition and content of refined tallow (without molecular distillation treatment) and separated tallow obtained in Examples 1–6

Claims

Claim 1: A separation method for improving the flavor of beef tallow and the content of unsaturated fatty acid, characterized in that refined beef tallow is balanced in a room temperature environment, then water bath heating is carried out until the beef tallow is completely transparent liquid, short-range molecular distillation treatment is carried out on the beef tallow completely transparent liquid, and the separated beef tallow is obtained, wherein the distillation temperature of short-range molecular distillation is 160–210°C.

Claim 2: The method according to Claim 1, wherein the equilibration period is not less than 30 minutes; the water temperature of the water bath heating is 50–55°C.

Claim 3: The method according to Claim 1, wherein the short-path molecular distillation treatment is carried out in a short-path molecular distillation instrument; the vacuum degree in the distillation cavity of the short-range molecular distillation instrument is lower than 0.1 MPa, the short-range molecular distillation instrument starts chilled water circulation, and the condensation temperature of the light phase component is 50–55°C.

Claim 4: The method according to Claim 1, wherein the feeding rate of short-path molecular distillation treatment is 50–55 drops/min, and the film scraping rotating speed is 200–250 r/min.

Claim 5: The method according to Claim 1, wherein the distillation temperature of short-path molecular distillation is 160–180°C.

Claim 6: The method according to Claim 5, wherein the mass ratio of unsaturated fatty acid in the separated beef tallow is more than or equal to 55%.

Claim 7: The method according to Claim 5, wherein the separated beef tallow has a content of fat flavor profile that is at least 1.5 times higher than the content of fat flavor profile in refined beef tallow.

Claim 8: The method according to Claim 5, wherein the separated tallow is characterized by a fat taste profile that is at least 40% higher than a refined tallow by a sensory evaluation score of fat taste obtained from experiments conducted with descriptive sensory analysis.

Summary of Technical Contribution

1. Novel Application of Molecular Distillation: The invention applies short-path molecular distillation specifically for the separation of beef tallow to achieve concurrent enrichment of unsaturated fatty acids and directional improvement of flavor.
2. Optimized Temperature Control: The invention identifies the critical temperature range (160–210°C) for molecular distillation of beef tallow, with 160–180°C being particularly preferred for optimal results.
3. Dual Optimization of Nutrition and Flavor: Demonstrates simultaneous improvement in both nutritional profile (increased unsaturated fatty acids) and sensory properties (enhanced flavor characteristics).
4. Scalable Melting Point Control: Creates a stepped melting point system (32.07–43.13°C) from a single raw material melting point (44.1°C), enabling tailored applications.
5. Comprehensive Characterization: Provides thorough analytical data including:
   • Fatty acid composition
   • Melting point behavior
   • Sensory evaluation
   • Aroma compound quantification via GC-MS
6. Comparative Validation: Multiple examples demonstrate the effect of varying distillation temperatures on product properties.

Conclusion

The present invention provides a separation method for improving beef tallow flavor and unsaturated fatty acid content using short-path molecular distillation technology developed by Shanghai Institute of Technology. The method successfully achieves:

• Increased unsaturated fatty acid content from 40.85 g/100g to 57 g/100g
• Enhanced fat flavor characteristic substances by 2–3 times
• Improved sensory scores by at least 40%
• Tailored melting points for different applications

The method is simple to operate, does not introduce chemical substances or cause thermal decomposition, and enables high-value utilization of beef tallow with "one material, multiple uses," making it suitable for various food processing applications including baking, hotpot condiments, and artificial butter production.

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