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CN113383958A - Soft capsule of krill oil - Google Patents

Soft capsule of krill oil Download PDF

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Publication number
CN113383958A
CN113383958A CN202010167591.7A CN202010167591A CN113383958A CN 113383958 A CN113383958 A CN 113383958A CN 202010167591 A CN202010167591 A CN 202010167591A CN 113383958 A CN113383958 A CN 113383958A
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parts
soft capsule
krill oil
water
oil
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Inventor
程刚
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Beijing Kang Lisheng Pharmaceutical Technology Development Co ltd
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Beijing Kang Lisheng Pharmaceutical Technology Development Co ltd
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/115—Fatty acids or derivatives thereof; Fats or oils
    • A23L33/12—Fatty acids or derivatives thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3481—Organic compounds containing oxygen
    • A23L3/3508—Organic compounds containing oxygen containing carboxyl groups
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3544—Organic compounds containing hetero rings
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3562—Sugars; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/358—Inorganic compounds
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/115—Fatty acids or derivatives thereof; Fats or oils
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Inorganic Chemistry (AREA)
  • Medicinal Preparation (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention relates to a soft capsule of krill oil, the soft capsule skin is composed of the following components by weight: 90-110 parts of gelatin; 40-50 parts of glycerol; 90-110 parts of water; 20-30 parts of sodium hyaluronate; 10-20 parts of maltitol; 0.05-0.15 parts of procyanidine; 0.02-0.03 part of lactic acid; 0.6-0.8 part of caramel pigment; 0.01-0.02 part of titanium dioxide; the content is composed of krill oil and vitamin E.

Description

Soft capsule of krill oil
Technical Field
The invention belongs to the technical field of medicines, and relates to a soft capsule of krill oil.
Background
The krill oil is extracted from Euphausia superba Dana, modern scientific researches show that the krill oil mainly contains rich biological active substances such as eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA), phospholipid, astaxanthin and the like, and clinical researches prove that the krill oil has effective curative effects on dyslipidemia, chronic inflammation and cognitive disorder. Therefore, health foods containing krill oil are becoming hot spots in the field of development of nutritional health foods.
The krill oil contains more than 38% phospholipids and a certain amount of astaxanthin. Because the phospholipid has bipolarity, one end is a head group, and the other end is a hydrophilic chain and a hydrophobic chain, the phospholipid can be mixed with fatty acid and water and enter a chylomicron membrane as a membrane component, and the chylomicron is released into blood and sent to the whole body, so that the bioavailability of DHA and EPA in krill oil is improved.
The soft capsule as one kind of health food is prepared through dissolving medicine and medicine extract in proper amount of liquid supplementary material and pressing or dropping into spherical or olive soft capsule. The product has the advantages of high bioavailability, quick absorption, capability of covering the unpleasant odor of the contents, small dosage, beautiful appearance, convenient carrying and the like, and is widely used in the field of health food. However, due to the complexity of the contents of the soft capsule and the mutual migration of the contents and the gelatin skin substances, the quality problems of the soft capsule, such as exceeding the disintegration time limit, oil leakage and the like, can also be caused.
The sodium hyaluronate has strong water absorbability, is widely applied to the field of cosmetics all the time, mainly has a good moisturizing effect, and is proved by research to be capable of improving skin moisture better than a control group and simultaneously has a certain antioxidation effect.
Compared with other preparations, the soft capsule prepared from the health food containing the krill oil has better isolation function, can isolate functional materials sensitive to light and oxygen from air, and prevents the contents from being oxidized. However, for soft capsule products containing krill oil as a content, water in the capsule shell is absorbed by phospholipids due to the hydrophilicity of the phospholipids in the krill oil. In addition, the existence of astaxanthin can increase the permeability of contents, accelerate the migration of phospholipid to water in the capsule skin, cause the hardening of the capsule, and the aging of the capsule skin leads to oil leakage.
Disclosure of Invention
The invention aims to overcome the defects and provide a soft krill oil capsule.
The soft capsule shell provided by the invention comprises the following components in parts by weight: 90-110 parts of gelatin; 40-50 parts of glycerol; 90-110 parts of water; 20-30 parts of sodium hyaluronate; 10-20 parts of maltitol; 0.05-0.15 parts of procyanidine; 0.02-0.03 part of lactic acid; 0.6-0.8 part of caramel pigment; 0.01-0.02 part of titanium dioxide.
Preferably, the soft capsule shell consists of the following components in parts by weight: 100 parts of gelatin; 45 parts of glycerol; 100 parts of water; 30 parts of sodium hyaluronate; 15 parts of maltitol; 0.05 part of procyanidine; 0.025 parts of lactic acid; 0.7 part of caramel pigment; 0.015 part of titanium dioxide.
The content of the soft capsule provided by the invention consists of krill oil and vitamin E, and preferably 99.8 parts by weight of krill oil and 0.2 part by weight of vitamin E.
Experimental example krill oil and vitamin E formulation optimization procedure
Since main functional components in krill oil are eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA), phospholipids and astaxanthin, which are all easily oxidized, an antioxidant vitamin E is added to the formula in order to ensure the quality of the product. In order to determine the proper vitamin E adding amount, different percentages of vitamin E are designed to be added, accelerated inspection is carried out for 27 days at the temperature of 60 ℃, and the peroxide value and the acid value of a finished product are respectively inspected and accelerated at different time, so that the proper vitamin E adding amount is determined, and the result is shown in table 1.
TABLE 1 screening of krill oil softgel vitamin E dosage
Figure BDA0002408008250000021
As can be seen from Table 1, the lower the peroxide value of the finished krill oil soft capsule at each time point of the accelerated test is, the higher the addition amount of vitamin E is, the better the antioxidant effect is. According to the use principle of the food additive, in order to reduce the addition of the antioxidant as much as possible and ensure the quality of the product, the quality requirement of the product can be met when the addition of the vitamin E is 0.2 percent by referring to the quality index of the soybean oil. Therefore, the formula of the product is determined that the addition amount of krill oil is 99.8%, and the addition amount of vitamin E is 0.2%.
According to the invention, sodium hyaluronate, maltitol, procyanidine and lactic acid are compounded to be used as a water-retaining agent, so that water in the soft capsule shell can be effectively locked, and the water is delayed from transferring to hydrophilic groups of phospholipid in krill oil, thereby delaying the aging of the capsule shell.
Meanwhile, sodium hyaluronate and water in the capsule skin form a compound, and the sodium hyaluronate can carry more than 500 times of water, so that the water in the capsule skin is prevented from transferring, and the water in the capsule skin of the soft capsule is kept within a certain range.
Maltitol has certain water retention property, has synergistic effect when used together with sodium hyaluronate, and can form hydrogen bond with hydroxyl and molecule at water loss part of dried biological molecule instead of hydrogen bond formed by water, and the formation of the hydrogen bond can inhibit protein from unfolding caused by dehydration deformation, so that human can maintain original mechanism of molecule without losing activity under water-deficient condition(1)。
Although the lactic acid can not directly keep water, the capsule skin can be kept under the weak acid condition, the formation of hyaluronic acid water molecule complexes is promoted, and the synergistic effect of the hyaluronic acid on keeping the water in the capsule skin is realized.
The procyanidin has strong oxidation resistance, and due to the special properties of gelatin, the procyanidin contains protein of metal ions, is easy to contact with air to cause oxidative discoloration, affects the color of the gelatin skin, can rapidly and effectively remove dissolved oxygen in the gelatin skin, and can prevent oil leakage due to oxidation hardening of the gelatin skin(1). Meanwhile, due to the existence of the antioxidant, the formation of aldehyde substances in the capsule shell is avoided, and the crosslinking aging phenomenon of the gelatin is effectively prevented(8)。
The addition of the pigment and the titanium dioxide can reduce the loss of EPA, DHA and other photosensitive materials in the soft capsule contents in the storage process and improve the shelf life of the soft capsule product.
The invention can prevent the water in the capsule shell from being absorbed by the phospholipid in the krill oil, thereby avoiding the hardening of the capsule and the oil leakage caused by the aging of the capsule shell, improving the quality stability of the soft capsule containing the krill oil and prolonging the storage period of the product.
Experimental example 1
In order to obtain the optimal formula of the soft capsule shell, orthogonal experimental design is adopted in the research process(9)The factors and levels are shown in Table 3, and sodium hyaluronate and malt are examined respectivelyThe krill oil soft capsule finished product is prepared when the addition of four factors, namely sugar alcohol, procyanidine and lactic acid is at three levels, and the optimal soft capsule shell formula is determined by observing the days for oil leakage of the finished product under the conditions that the temperature is 37.5 ℃ and the humidity is 75% in the accelerated test condition of the health food.
TABLE 3 levels of factors
Figure BDA0002408008250000031
TABLE 4 results of orthogonal experiments
Figure BDA0002408008250000032
From the results of the orthogonal experiments and the range analysis in table 4, the following factors affecting the number of days for oil leakage of the soft capsules can be obtained in sequence: a is more than B and more than C is more than D, and the optimal formula of the soft capsule shell is as follows: a. the3B2C1D2。
Because the optimal soft capsule proportion is not in the orthogonal experiment, three batches of soft capsule finished products are prepared according to the optimal soft capsule skin formula obtained by the orthogonal experiment, the number of days of oil leakage of the soft capsule finished products is examined, and the result of the orthogonal experiment is verified.
Results of the Table verification test
Figure BDA0002408008250000041
And (3) knotting: according to results of orthogonal experiments and verification tests, the soft capsule skin comprises the following components in parts by weight: 100 parts of gelatin; 45 parts of glycerol; 100 parts of water; 30 parts of sodium hyaluronate; 15 parts of maltitol; 0.1 part of procyanidine; 0.025 parts of lactic acid; 0.7 part of pigment; 0.015 part of titanium dioxide. The soft capsule finished product has the longest oil leakage days under the accelerated test condition, and meets the requirement of the quality guarantee period of the common soft capsule finished product.
Experimental example 2 method for measuring docosahexaenoic acid (DHA) in krill oil
Docosahexaenoic acid (DHA) is one of main functional components in krill oil, in order to accurately analyze the content of the DHA in the krill oil, reference is made to the current commonly used national detection standard of DHA, GB 28404-.
Table DHA content detection method groping condition and result
Figure BDA0002408008250000042
From the results in the table, firstly, referring to the method of GB 28404 completely, using PEG column and the gas chromatography temperature-rising program in GB 28404, it was found that the actual detection result of the DHA content in krill oil is 1 times higher than the theoretical value, and it may be that the actual detection result is higher because DHA methyl ester is not separated from other components, and it is seen that GB 28404 is not suitable for analyzing DHA in krill oil. And secondly, examining the applicability of GB26400 to the DHA content in krill oil, and finding that DHA methyl ester and the previous peak can not be separated from each other by using a DB-5ms column and adopting the temperature programming condition in the GB26400 method. Thus, considering replacing the less polar column DB-35 and using the temperature programmed conditions of the GB26400 method, it was found that DHA methyl ester was not retained in the column and the temperature programmed for possible analytical reasons was not high enough. Thus, the final temperature program was adjusted from 250 ℃ to 290 ℃ and DHA methyl ester was found to be retained and quantitatively accurate.
Experimental example 3: capsule skin formulation under different embodiments
Figure BDA0002408008250000051
Detailed Description
Example 1
The invention is composed of the capsule skin components of the soft capsule according to the weight ratio of the specific example N-1
The preparation method comprises the following steps:
1. preparation of content material liquid: 99.8 parts of krill oil and 0.2 part of vitamin E, homogenizing and stirring for about 1hr, and degassing to obtain a content material liquid;
2. preparing glue solution: weighing purified water and glycerol according to a formula proportion, mixing, preheating to about 50 ℃, adding gelatin, caramel pigment and titanium dioxide, heating to 70 ℃, stirring for 1h, melting gelatin, adding sodium hyaluronate, maltitol, procyanidine and lactic acid according to the formula proportion, stirring for 1-2h according to the weight ratio of the capsule skin components of the soft capsule in the embodiment N ═ 1, vacuumizing, filtering (100 mesh sieve), standing, and preserving heat below 60 ℃ to obtain a gelatin solution;
3. pelleting: making the content material liquid and the glue solution into soft capsules at the temperature of 18-26 ℃ and the relative humidity of 25-65 percent to obtain the soft capsules, wherein each capsule is 0.5 g;
4. shaping: the time is 1-2 hours, the temperature is 18-26 ℃, and the relative humidity is 25% -65%;
5. and (3) drying: the temperature is 20-30 ℃, the relative humidity is 15-45%, and the time is 48-72 hours;
6. selecting pills: removing the capsules which do not meet the requirements;
7. wiping pills: the pills are rubbed with 75 percent of alcohol,
removing oil stains on the surface of the capsule;
8. cooling pills: the temperature is 18-26 ℃, the relative humidity is 45-65%, and the time is 1-2 h;
9. inner packaging: 60 granules/bottle;
example 2
The invention is formed according to the weight ratio of the capsule skin components of the soft capsule of the specific embodiment N-2.
Example 3
The invention is formed according to the weight ratio of the capsule skin components of the soft capsule of the specific embodiment N-3.
Example 4
The invention is formed according to the weight ratio of the capsule skin components of the soft capsule of the specific embodiment N-4.
Example 5
The soft capsule shells of the soft capsules of examples 1 to 4 are used for preparing the krill oil soft capsules, and the quality standard of the krill oil meets the new krill oil food raw material bulletin (3) issued by the State health Commission. The weight of the content is 0.5 g/granule, and the days for finding oil leakage and procyanidin days are examined under the conditions of accelerated test temperature of 37.5 deg.C and humidity of 75% of the health food.
Days for oil leakage of soft capsule finished product in different embodiments
Figure BDA0002408008250000061
Example 6
The content of docosahexaenoic acid (DHA) in each of 10 soft capsules of examples 1 to 4 was measured by placing each 10 soft capsules on an oil-absorbing paper (10CM ) at 37.5 ℃ and 75% humidity, replacing the oil-absorbing paper once a day, and measuring the content of DHA in the replaced oil-absorbing paper.
Sample treatment: the oil absorption paper is smashed and mixed evenly to obtain 1g (accurate to 0.001g) of a sample to be detected, the sample is added into a 50mL colorimetric tube, 8mL of water is added, and 10mL of hydrochloric acid is added after even mixing. And (3) putting the colorimetric tube into a water bath at 75 ℃, and mixing the colorimetric tube once every 5-10 min by using a vortex mixer until the sample is completely hydrolyzed, wherein the time is about 45 min. The cuvette was removed, 10mL of ethanol was added, and mixed. After cooling to room temperature, the mixture was transferred into a 100mL stoppered measuring cylinder, the cuvette was washed with 25mL absolute ethyl ether in portions, and the mixture was poured into the measuring cylinder and shaken with a stopple for 1 min. Adding 25mL petroleum ether, shaking with a sealed plug for 1min, standing for 30min, separating the layers, and filtering the organic layer into a concentration bottle over anhydrous sodium sulfate (about 5 g). Adding 25mL of anhydrous ether, shaking for 1min, adding 25mL of petroleum ether, shaking for 1min, standing, layering, filtering the organic layer with anhydrous sodium sulfate (about 5g), adding 25mL of anhydrous ether … …, standing, layering, and drying under reduced pressure at 45 deg.C. Dissolving the concentrate with n-hexane for several times, transferring to a 25mL volumetric flask, fixing the volume, and shaking up to obtain the solution to be detected.
Methyl esterification treatment: sucking a liquid to be tested (2.0mL to 10mL test tubes with plug scales, adding 2.0mL potassium hydroxide methanol solution, immediately moving to a vortex mixer, shaking and mixing for 5min, standing for 5min, adding 6mL distilled water, shaking up and down for 0.5min, standing for layering, sucking a lower layer liquid, discarding, repeatedly washing with a small amount of distilled water, discarding a water layer with a suction tube until the liquid is neutral (centrifuging at 4000r/min for 10min if the organic phase has emulsification), and sucking a n-hexane layer to be tested on a computer.
Reference conditions for gas chromatography
The chromatographic column is a bonded cross-linked polyethylene glycol stationary phase, has the column length of 30m, the inner diameter of 0.32mm and the film thickness of 0.5 mu m or the chromatographic column with the same performance.
Temperature of the column oven: the initial temperature is 180 ℃, the temperature is increased to 220 ℃ at the speed of 10 ℃/min, then the temperature is increased to 290 ℃ at the speed of 8 ℃/min, and the temperature is kept for 13 min.
Sample inlet temperature: 250 ℃; the sample amount is 1 mu L, and the split ratio is 20: 1.
FID detector temperature: 270 ℃.
Carrier gas: high-purity nitrogen with the flow rate of 1.0mL/min and tail blowing of 25 mL/min.
Hydrogen gas: 40 mL/min; air 450 mL/min.
And (3) preparing a standard curve: injecting 1 μ L of standard series solutions with various concentrations into gas chromatograph, measuring corresponding peak area or peak height,
and (4) drawing a standard curve by taking the concentration of the standard working solution as an abscissa and taking the peak area or the peak height as an ordinate.
Determination of test solutions: injecting 1 mu L of sample solution to be detected into a gas chromatograph, determining the nature of the sample solution by retention time, measuring peak area or peak height, and obtaining the component concentration of each fatty acid methyl ester in the solution to be detected according to a standard curve.
Example 7
10 soft capsules of examples 1 to 4 were used, each containing 0.5 g/capsule of the content, and the content was measured by placing each 10 soft capsules on an oil-absorbing paper (10CM ) at 37.5 ℃ and 75% humidity, replacing the oil-absorbing paper once a day, and measuring the content of procyanidin on the replaced oil-absorbing paper.
Procyanidine detection method
1. Chromatographic conditions are as follows:
a chromatographic column:
Figure BDA0002408008250000071
c18 Pyramid, 250 mm. times.4.6 mm, 5 μm; mobile phase: methanol-1.44% aqueous acetic acid 25:75 (by volume); flow rate: 0.8 ml/min; column temperature: 25 ℃; corona Ultra CAD detector atomization chamber temperature: 35 ℃; sample introduction amount: 10 μ L.
2. Preparation of control solutions
Respectively and precisely weighing 30mg of procyanidine standard substance in a 25mL volumetric flask, adding methanol to dissolve, fixing the volume to a scale, and shaking up for later use.
3. And preparing a test solution.
Sample treatment: the method comprises the steps of crushing and uniformly mixing oil absorption paper to obtain 1g (accurate to 0.001g) of a sample to be detected, adding methanol into a 25mL volumetric flask to dissolve the sample and fix the volume to a scale, carrying out ultrasonic treatment for 30 minutes, shaking up, filtering, and fixing the volume to 25mL to obtain a standby solution;
mixing the solutions, collecting 1mL, adding 6mL hydrochloric acid-n-butanol, 200 μ L2% ferric ammonium sulfate, boiling in water bath for 40min, cooling in ice water bath, diluting to 25mL, shaking, and filtering with 0.22 μm filter membrane to obtain sample solution;
investigation of linear relationship
Preparing a procyanidin standard curve: precisely preparing control solutions with concentrations of 15, 30, 60, 120 and 150 μ g/mL respectively, and shaking up. Separately injecting samples, and measuring peak areas. And (3) taking the concentration (C) as a horizontal coordinate and the peak area (A) as a vertical coordinate, drawing a standard curve to obtain a regression equation: a is 0.006C-0.031, R2 is 0.998
The sample injection of the test solution shows that the proanthocyanidin retention time is 10.8min, the retention time is stable, and the peak pattern is better.
The days of oil leakage is found to be in a correlation relationship with the days of procyanidine discovery, so the procyanidine detection method can be used for detecting the soft capsules containing the krill oil.
Reference to the literature
Effect of antarctic krill oil on human health;
the bulletin of the health department-krill oil.

Claims (1)

1. A soft capsule of krill oil: the soft capsule shell comprises the following components in parts by weight: 90-110 parts of gelatin; 40-50 parts of glycerol; 90-110 parts of water; 20-30 parts of sodium hyaluronate; 10-20 parts of maltitol; 0.05-0.15 parts of procyanidine; 0.02-0.03 part of lactic acid; 0.6-0.8 part of caramel pigment; 0.01-0.02 part of titanium dioxide; the content is composed of krill oil and vitamin E.
CN202010167591.7A 2020-03-11 2020-03-11 Soft capsule of krill oil Pending CN113383958A (en)

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CN115969037A (en) * 2023-03-02 2023-04-18 贵州恒生源农业开发有限公司 Production process of oil tea soft capsules

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