Rapid prediction method of rancidity for high-temperature-intolerant powdered products containing oil and fat

Abstract

This invention relates to a rapid prediction method for the spoilage period of heat-sensitive, oil-containing powdered products. The method includes: measuring the shelf life (t) of pure oil products from different manufacturers with the same shelf life; measuring the OSI value of the oil at 120°C and calculating the average value (a); placing the oil-containing powdered products in ovens at different temperatures for fortification, and determining the highest fortification temperature (T) at which browning does not occur; taking pure oil with an OSI value of a ± 0.1 h and measuring the sensory spoilage period (d days) of the pure oil at T°C, and calculating the average peroxide value rate (V1); fortifying the oil-containing powdered products at T°C for d days; taking oil-containing powdered samples before and after fortification, extracting them with an organic solvent to obtain the extracted oil before and after fortification, and calculating the average peroxide value rate (V2); if V2 ≤ V1, then the predicted spoilage period of the oil-containing powdered products is ≥ t. This invention provides a simple and highly accurate method.

Description

Technical Field

[0001] This invention relates to the food industry, and more specifically, this application relates to a method for rapidly predicting the spoilage period of heat-sensitive, oil-containing powdered products. Background Technology

[0002] Among related technologies, the commonly used methods for predicting the shelf life of pure oil products include the following: oven drying method, AOM method, Rancimat method, etc. These methods measure the limits of evaluation parameters (POV value, OSI value, etc.) of pure oils at different temperatures, and then use extrapolation to calculate the shelf life of oil samples at room temperature.

[0003] In the food industry, predicting the shelf life of oil-containing powdered products has always been a technical challenge. Unlike pure oil products, which can be fortified by increasing temperature to accelerate rancidity and shorten fortification time, oil-containing powdered products (which are not heat-resistant) undergo chemical reactions during high-temperature fortification, leading to prediction failures. Conversely, storing them at room temperature results in excessively long shelf lives, significantly limiting new product development cycles and increasing R&D costs. Summary of the Invention

[0004] The present invention aims to at least partially solve one of the technical problems in the related art. To this end, the embodiments of the present invention provide a relatively accurate method for predicting the rancidity cycle of oil-based powdered products that are prone to reaction at high temperatures (≥70°C).

[0005] The embodiments of the present invention adopt the following technical solutions:

[0006] This invention provides a method for rapidly predicting the spoilage period of heat-sensitive, oil-containing powdered products, comprising the following steps:

[0007] (1) Measure three or more pure oil products of the same type from different manufacturers that are purchased from the market, with consistent shelf life labels and production dates close to purchase dates. The shelf life is recorded as t. The oxidation induction period of the oil at 120℃ is measured using an oil oxidation stability analyzer, i.e., the OSI value. The average value is calculated and recorded as a (the a value is used as a reference for the shelf life t at room temperature).

[0008] (2) Place the oil-containing powdered products in ovens at different temperatures for 3-5 days to strengthen them, with a temperature interval of 10℃. The highest strengthening temperature that does not cause browning is taken as the optimal strengthening temperature T.

[0009] (3) Take the OSI value as a±0.1h for pure oil, measure the sensory rancidity period of pure oil at T℃ and record it as d days, measure the initial peroxide value P0 of pure oil, measure the peroxide value P1 of pure oil after d days at T℃, and calculate the average peroxide value rate V1=(P1-P0) / d of pure oil.

[0010] (4) Place the oil-containing powdered product in an oven and heat it at T℃ for d days, then remove it for use;

[0011] (5) Take the oil-containing powder samples before and after strengthening, add an organic solvent, wherein the organic solvent is one of diethyl ether, petroleum ether, acetone or dichloromethane, wherein the mass ratio of the powder sample to the organic solvent is 1:(2-3), let stand for 24 hours, filter with filter paper, take the liquid phase, and place the extract at 40-60℃ for rotary evaporation to obtain the oil before strengthening and the oil after strengthening.

[0012] (6) Measure the peroxide value of the extracted oil before fortification and record it as P0'. Measure the peroxide value of the extracted oil after fortification and record it as P2. Calculate the average peroxide value rate V2=(P2-P0') / d.

[0013] If V2≤V1, then the predicted spoilage period for powdered products containing oil is ≥t.

[0014] In some embodiments, in step (2), the different temperatures are selected as 40°C, 50°C, 60°C, 70°C, 80°C, or 45°C, 55°C, 65°C.

[0015] In some embodiments, the method for determining the sensory rancidity period of pure oil at T℃ in step (3) is as follows: place the pure oil in a triangular glass bottle, cover the bottle mouth with 6 layers of plain white cloth, tie the mouth with cotton rope, place it in a constant temperature oven at T℃, until sensory rancidity is observed, and record the time as d days.

[0016] In some embodiments, the sensory evaluation of rancidity is performed as follows: a sensory evaluation team composed of multiple sensory evaluation professionals (5 or more people) scores the samples by direct smelling, and the average score is calculated. When the average score is ≤3 points, the product is determined to be rancid; otherwise, it is rancid. The scoring rules are: no rancid odor: 0-3 points; mild rancid odor: 4-6 points; moderate rancid odor: 7-8 points; severe rancid odor: 9-10 points.

[0017] In some embodiments, in step (5), the mass ratio of the powdered sample to the organic solvent is 1:2.

[0018] Preferably, in step (5), the organic solvent is diethyl ether or petroleum ether, more preferably, the organic solvent is petroleum ether.

[0019] In some embodiments, the fats include, but are not limited to, one or more of lard, beef tallow, chicken fat, or mutton fat.

[0020] The present invention has the following advantages and beneficial effects:

[0021] (1) The method of the present invention is for powdered products containing oils that are prone to high-temperature reactions. Compared with related technologies, the method of the present invention is a simpler and more accurate method for predicting the shelf life of products that spoilage.

[0022] The method of this invention avoids the currently commonly used fortification method, which directly places the oil-containing powdered product at a high temperature for fortification. Although the time is short, the presence of sugars and amino acids in the product causes the oil to participate in the Maillard reaction, resulting in fortification failure. It also avoids the problem of placing the powder at a low temperature for fortification in related technologies, which greatly prolongs the fortification cycle. Moreover, the method of this invention is more accurate and avoids the human error of sensory judgment of product failure during the fortification process.

[0023] (2) The method of the present invention utilizes the evaluation and analysis of the OSI value of oils to determine the standard sample of pure oils, laying the foundation for the prediction of the shelf life of powdered products containing oils. Attached Figure Description

[0024] Figure 1 This describes the color change of the powdered product containing refined chicken oil in Example 1 of the present invention after being fortified at different temperatures for 3 days.

[0025] Figure 2 This is a spectrum showing the OSI value of refined chicken oil (sample 2) from a commercially available manufacturer, as described in Example 1 of this invention.

[0026] Figure 3 This is a spectrum showing the OSI value of chicken bone oil (sample 2) from a commercially available manufacturer in Example 2 of the present invention. Detailed Implementation

[0027] The embodiments of the present invention are described in detail below. These embodiments are exemplary and intended to explain the present invention, and should not be construed as limiting the present invention.

[0028] This invention provides a method for rapidly predicting the spoilage period of heat-sensitive, oil-containing powdered products, comprising the following steps:

[0029] (1) Measure three or more pure oil products of the same type from different manufacturers that have the same shelf life label and production date and purchase date. The shelf life is recorded as t. The oxidation induction period of the oil at 120℃ is measured by an oil oxidation stability analyzer, i.e., the OSI value. The average value is calculated and recorded as a (a is used as a reference for the shelf life t at room temperature).

[0030] (2) Place the oil-containing powdered products in ovens at 40℃, 50℃, 60℃, 70℃, and 80℃ (or 45℃, 55℃, and 65℃) for 3-5 days to strengthen them. The highest strengthening temperature that does not cause browning is taken as the optimal strengthening temperature T.

[0031] (3) Take the OSI value as a±0.1h for pure oil, measure the sensory rancidity period of pure oil at T℃ and record it as d days, measure the initial peroxide value P0 of pure oil, measure the peroxide value P1 of pure oil after d days at T℃, and calculate the average peroxide value rate V1=(P1-P0) / d of pure oil.

[0032] The method for determining the sensory rancidity period of pure oil at T℃ is as follows: Place the pure oil in a triangular glass bottle, cover the bottle mouth with 6 layers of plain white cloth, tie the mouth with cotton rope, and place it in a constant temperature oven at T℃ until sensory rancidity is observed. The time is recorded as d days.

[0033] The sensory evaluation process for rancidity is as follows: A sensory evaluation team of 7 professionals will directly smell and score the samples, and the average score will be calculated. If the average score is ≤3, the product is considered rancid; otherwise, it is rancid. The scoring rules are as follows: No rancid odor: 0-3 points; Slight rancid odor: 4-6 points; Moderate rancid odor: 7-8 points; Severe rancid odor: 9-10 points.

[0034] (4) Place the oil-containing powdered product in an oven and heat it at T℃ for d days, then remove it for use;

[0035] (5) Take the oil-containing powder samples before and after strengthening, respectively, and add an organic solvent, wherein the organic solvent is one of diethyl ether, petroleum ether, acetone or dichloromethane, and the mass ratio of powder sample to organic solvent (extractant) is 1:2. Filter with filter paper, take the liquid phase, and place the extract at 40-60℃ for rotary evaporation to obtain the oil before strengthening and the oil after strengthening;

[0036] (6) Measure the peroxide value of the extracted oil before fortification and record it as P0'. Measure the peroxide value of the extracted oil after fortification and record it as P2. Calculate the average peroxide value rate V2=(P2-P0') / d.

[0037] If V2≤V1, then the predicted spoilage period for powdered products containing oil is ≥t.

[0038] In this embodiment of the invention,

[0039] OSI value determination method: Refer to GB / T 21121-2007

[0040] Method for determining peroxide value: Refer to GB5009.227-2016

[0041] Methods for calculating oil extraction rate:

[0042] Extraction rate (%) = m1 / m2

[0043] m1 represents the mass of oil extracted from the powder matrix by using an organic solvent to extract the oil from the externally added oil, and m2 represents the total mass of oil actually added to the powder matrix.

[0044] In this embodiment of the invention, the strengthening time of 3-5 days is selected in step S2. This is based on the applicant's findings during the experiment on strengthening tests of different oil-containing powder products. If the color of the sample does not change significantly after being strengthened at a certain temperature for more than 3 days, it can be determined that browning will not occur at that temperature.

[0045] Among them, powdered sample 1# is chicken powder flavoring, which contains chicken fat.

[0046] Among them, powder sample 2# is thermally reacted chicken powder, which contains chicken fat.

[0047] Among them, powdered sample #3 is beef powder flavoring, which contains beef fat.

[0048] Among them, powdered sample #4 is thermally reacted beef powder, which contains beef fat.

[0049] Table 1

[0050]

[0051] Table 2

[0052]

[0053]

[0054] Table 3

[0055]

[0056] Table 4

[0057]

[0058] Example 1:

[0059] A method for predicting the spoilage shelf life of powdered products containing refined chicken fat includes the following steps:

[0060] (1) The shelf life of refined chicken oil from four manufacturers on the market was measured at room temperature for one year. The induction period of the oil at 120℃, i.e., the OSI value, was measured. The average value was calculated and the average peroxide value was 2.3h. This value can be used as a reference sample for refined chicken oil with a shelf life of 12 months (at room temperature).

[0061] Table 5

[0062] Refined chicken fat sample Sample 1 Sample 2 Sample 3 Sample 4 Average value approximately OSI value 2.15 2.30 2.32 2.41 2.3

[0063] (2) Place a powdered product containing refined chicken fat in an oven at 40℃, 50℃, 60℃, 70℃, and 80℃ for 3 days for intensive treatment, respectively. See Figure 1 The powder product did not change color when strengthened at 40℃ and 50℃, but the color gradually deepened above 60℃. Therefore, the optimal strengthening temperature was set at 50℃.

[0064] (3) Take refined chicken oil (OSI value of 2.3±0.1h) and place it in a triangular glass bottle. Cover the bottle mouth with 6 layers of white cloth, tie the mouth with cotton rope, and place it in a constant temperature oven. The sensory decay period of the refined chicken oil at 50℃ is 12 days. The initial peroxide value of the refined chicken oil is 0.01g / 100g. The peroxide value of the refined chicken oil after 12 days at 50℃ is 1.45g / 100g. The average peroxide rate of the refined chicken oil is calculated to be V1=0.12g / 100g·d.

[0065] (4) Place the powdered product containing refined chicken oil in an oven and heat it at 50°C for 12 days. Then take it out and set it aside for use.

[0066] (5) Take the oil-containing powder samples before and after strengthening, add petroleum ether, extract by standing for 24 hours at a mass ratio of 1:2, filter with filter paper, take the liquid phase, and place the extract at 40℃ for rotary evaporation to obtain the oil before strengthening and the oil after strengthening.

[0067] (6) The peroxide value of the extracted oil before fortification was measured to be 0.03 g / 100 g, and the peroxide value of the extracted oil after fortification was measured to be 1.11 g / 100 g. The average peroxide value rate V2 was calculated to be 0.09 g / 100 g·d.

[0068] If V2 < V1, then the shelf life of the powdered product containing refined chicken fat can be determined to be 1 year.

[0069] The embodiments of the present invention also determined the effect of different extraction solvents on the antioxidant properties of refined chicken oil in the powdered sample containing oil in step (5), as shown in Table 6.

[0070] Table 6

[0071]

[0072] As shown in Table 6, using diethyl ether or petroleum ether as an organic solvent has virtually no effect on the antioxidant properties of the oil. However, when acetone is used as the extraction solvent, the higher temperature required for rotary evaporation may be the main reason for the decrease in the OSI value of refined chicken oil. In addition, the extraction rates of the solvents for refined chicken oil from high to low are petroleum ether > dichloromethane > acetone > diethyl ether. Therefore, considering all factors, petroleum ether is the best extraction solvent for refined chicken oil.

[0073] Example 2:

[0074] A method for predicting the spoilage shelf life of powdered products containing chicken bone oil includes the following steps:

[0075] (1) Chicken bone oil samples from four manufacturers on the market, with a shelf life of 6 months when stored at room temperature, were tested for the induction period of the oil at 120℃, i.e., the OSI value. The average value was calculated and the average peroxidation value was 1.5h. This value can be used as a reference for chicken bone oil with a shelf life of 6 months (stored at room temperature).

[0076] Table 7

[0077] Chicken bone oil sample Sample 1 Sample 2 Sample 3 Sample 4 Average value approximately OSI value 1.44 1.51 1.45 1.61 1.5

[0078] (2) A powdered product containing chicken bone oil was placed in an oven at 45℃, 55℃ and 65℃ for 3 days. The color of the powdered product did not change at 45℃ and 55℃, but the color gradually deepened above 65℃. Therefore, the optimal strengthening temperature was set to 55℃.

[0079] (3) Take chicken bone oil (OSI value is 1.5±0.1h), put it in a triangular glass bottle, cover the bottle mouth with 6 layers of white cloth, tie the mouth with cotton rope, and put it in a constant temperature oven. The sensory decay period of the chicken bone oil at 55℃ is 7 days.

[0080] The initial peroxide value of the chicken bone oil was determined to be 0.02 g / 100 g; the peroxide value of the chicken bone oil after being placed at 55℃ for 7 days was determined to be 1.49 g / 100 g; the average peroxide rate of the chicken bone oil was calculated to be V1 = 0.21 g / 100 g·d.

[0081] (4) Weigh out the powdered product containing chicken bone oil, place it in an oven, strengthen it at 55℃ for 7 days, and then take it out for use;

[0082] (5) Weigh the powdered sample containing chicken bone oil before and after strengthening, add petroleum ether, extract for 24 hours at a mass ratio of 1:2.5, filter with filter paper, take the liquid phase, and place the extract at 40℃ for rotary evaporation to obtain the extracted oil before strengthening and the extracted oil after strengthening.

[0083] (6) The peroxide value of the extracted oil before fortification was measured to be 0.01 g / 100 g, and the peroxide value of the extracted oil after fortification was measured to be 1.27 g / 100 g. The average peroxide value rate V2 was calculated to be 0.18 g / 100 g·d.

[0084] V 2＜ V1 indicates that the shelf life of the powdered product containing chicken bone oil can be determined to be 6 months.

[0085] Validation of the prediction method model

[0086] Using the above method, the shelf life of five powdered products containing chicken fat (without other oils) was determined, and the products were placed at room temperature to observe the sensory decay period.

[0087]

[0088]

[0089] The experimental results above show that the constructed prediction method model is feasible for predicting the spoilage of powdered oil-containing products that are prone to high-temperature reactions.

[0090] In this invention, the terms "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., refer to a specific feature, structure, material, or characteristic described in connection with that embodiment or example, which is included in at least one embodiment or example of the invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0091] Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention. Those skilled in the art can make changes, modifications, substitutions and variations to the above embodiments within the scope of the present invention.

Claims

1. A method for rapidly predicting the spoilage period of heat-sensitive, oil-containing powdered products, characterized in that, Includes the following steps: (1) Determine the shelf life of pure oil products of the same type from three or more different manufacturers, with consistent shelf life markings and production dates close to purchase dates. Record the shelf life as t. Use an oil oxidation stability analyzer to measure the oxidation induction period of the oil at 120℃, i.e., the OSI value, calculate the average value, and record it as a. The value of a is used as a reference for the shelf life t at room temperature. (2) Place the oil-containing powdered products in ovens at different temperatures for 3-5 days for strengthening, with a temperature interval of 10℃. The highest strengthening temperature that does not cause browning is taken as the optimal strengthening temperature T. (3) Take pure oil with an OSI value of a ± 0.1 h, determine the sensory rancidity period of the pure oil at T℃ and record it as d days, determine the initial peroxide value P0 of the pure oil, determine the peroxide value P1 of the pure oil after being placed at T℃ for d days, and calculate the pure oil. Average peroxide value rate V1 = (P1 - P0) / d; (4) Place the oil-containing powdered product in an oven and heat it at T℃ for d days, then remove it for use; (5) Take the oil-containing powder samples before and after strengthening, add an organic solvent, wherein the organic solvent is one of diethyl ether, petroleum ether, acetone or dichloromethane, wherein the mass ratio of the powder sample to the organic solvent is 1:(2-3), let stand for 24 hours, filter with filter paper, take the liquid phase, and place the extract at 40-60℃ for rotary evaporation to obtain the oil before strengthening and the oil after strengthening. (6) Measure the peroxide value of the extracted oil before fortification and record it as P0'. Measure the peroxide value of the extracted oil after fortification and record it as P2. Calculate the average peroxide value rate V2 = (P2 - P0') / d. If V2≤V1, then the predicted spoilage period for powdered products containing oil is ≥t.

2. The method for rapid prediction of the spoilage period of heat-sensitive, oil-containing powdered products according to claim 1, characterized in that, In step (2), the different temperatures are selected as 40℃, 50℃, 60℃, 70℃, 80℃, or 45℃, 55℃, 65℃.

3. The method for rapid prediction of the spoilage period of heat-sensitive, oil-containing powdered products according to claim 1, characterized in that, In step (3), the method for determining the sensory rancidity period of pure oil at T℃ is as follows: place the pure oil in a triangular glass bottle, cover the bottle mouth with 6 layers of plain white cloth, tie the mouth with cotton rope, and place it in a constant temperature oven at T℃ until sensory rancidity is observed. The time is recorded as d days.

4. The method for rapid prediction of the spoilage period of heat-sensitive, oil-containing powdered products according to claim 3, characterized in that, The sensory evaluation process for rancidity is as follows: A sensory evaluation team composed of multiple sensory evaluation professionals will directly smell and score the samples, summing the scores and taking the average. When the average score is ≤3 points, the product is determined to be rancid; otherwise, it is rancid. The scoring rules are: no rancid odor: 0-3 points; mild rancid odor: 4-6 points; moderate rancid odor: 7-8 points; severe rancid odor: 9-10 points.

5. The method for rapid prediction of the spoilage period of heat-sensitive, oil-containing powdered products according to claim 1, characterized in that, In step (5), the mass ratio of the powdered sample to the organic solvent is 1:

2.

6. The method for rapid prediction of the spoilage period of heat-sensitive, oil-containing powdered products according to claim 1, characterized in that, In step (5), the organic solvent is diethyl ether or petroleum ether.

7. The method for rapid prediction of the spoilage period of heat-sensitive, oil-containing powdered products according to claim 6, characterized in that, The organic solvent is petroleum ether.

Images