TW201424778A - Sterilization method for powder and particulate substance - Google Patents

Abstract

The invention is an apparatus for the sterilization method of the powder and particulate problem by supercritical fluids. The sterilized method was applied to powder and particulate with a supercritical sterilization fluid at 20 to 120 minutes of contact. Among of them, the supercritical sterilization fluid system containing a weight percentage of 0.1 to 1.0% ethanol and 0.1 to 0.5% of the acetic acid in the supercritical carbon dioxide fluid (SC-CO2). The operating temperature of the fluid of the supercritical carbon dioxide is 40 to 60 DEG C, and operating pressure was used with per square inch of 1500 to 3000 pounds.

Description

Sterilization method for powder granules

The present invention relates to a method for sterilizing powdery granules, and more particularly to sterilizing the heat-sensitive powder granules by supercritical carbon dioxide fluid.

The sterilization method of the conventional food or medicine, including chemical sterilization, heat treatment or ultraviolet sterilization, according to the type or characteristics of the food or medicine, further selecting different sterilization methods, however, among many types of foods or medicines, Further, it is most difficult to sterilize powdery granules having a heat-sensitive component. In other words, a powder granule refers to a food or a drug which is formed into a stacked structure from a powder or a granular form, for example, if it contains A physiologically active enzyme powder, a lactic acid bacterial powder, a Chinese herbal medicine powder, or a pharmacological component or a strain coated or preserved with a microlipid.

1. When the heat-sensitive powder granules are treated by the chemical sterilization method, the chemical bactericide is usually added to the powder granules in an appropriate ratio, and the chemical bactericide remains, and other toxic substances are derived and free radicals are formed. In addition, the chemical bactericide also destroys the heat-sensitive active ingredient and renders its physiological activity ineffective.

2. When the heat sensitive powder granules are sterilized by heat treatment, the powder granules are usually sterilized at a temperature of 72 ° C or higher under moist heat conditions, at which time the heat sensitive component of the powder granules For example, pigments may be discolored due to heat treatment or cause browning, or heat-sensitive enzymes or pharmacological ingredients may be inactivated due to heat treatment.

3. When the above-mentioned powdery granules having heat-sensitive components are treated by ultraviolet sterilizing, although ultraviolet light can kill microorganisms, however, due to the stacked state of the powder granules, ultraviolet rays may be irradiated to the dead angles, and The bactericidal effect of the whole powder granules is not complete.

In summary, it is necessary to provide a sterilization method suitable for powdery granules having heat-sensitive components, so as to improve the sterilization mode of conventional foods or drugs without affecting the active ingredients or pharmacological properties thereof. Powder granules are sterilized.

SUMMARY OF THE INVENTION A primary object of the present invention is to provide a sterilizing method for powder granules which can be applied to sterilization of powder granules having a heat sensitive component without damaging the heat sensitive component.

A second object of the present invention is to provide a method for sterilizing powder granules which is capable of removing the amount of environmental microorganisms on the surface of the powder granules.

In order to achieve the foregoing object, the technical content of the present invention and the effects achievable by the technical means include: a sterilization method for powder granules, which is a powder granule and a super The critical sterilizing fluid is contacted for at least 20 minutes, preferably 20 to 120 minutes, wherein the supercritical sterilizing flow system comprises a supercritical carbon dioxide fluid having a weight percentage of 0.1-1.0% ethanol and 0.1-0.5% acetic acid, the supercritical The operating temperature of the carbon dioxide fluid is 40 to 60 ° C and the operating pressure is 1500 to 3000 pounds per square inch (pounds per square inch; psi).

In the method for sterilizing powder granules, when the powder granules are in contact with a supercritical sterilizing fluid, the weight ratio of the powder granules to the supercritical sterilizing fluid is preferably 1: 1~1:3.

In the method for sterilizing powder granules, the powder granules may be selectively contacted with the supercritical sterilizing fluid by dynamic sterilizing treatment, the powder granules and a fixed weight supercritical sterilizing fluid. At the time of contact, a new supercritical sterilizing fluid is supplemented at an infusion rate of 20 to 100 ml per minute to replace a portion of the supercritical sterilizing fluid that has been in contact with the powder granules.

In the method for sterilizing powder granules, when the powder granule is green papaya powder, the weight ratio of the green papaya powder to the supercritical sterilizing fluid is preferably 1:1.5, wherein the super The critical sterilizing fluid may be selected as a supercritical carbon dioxide fluid containing 0.5% by weight of ethanol and 0.5% of acetic acid. The operating pressure of the supercritical carbon dioxide fluid is preferably 1500 psi per square inch, and the operating temperature is preferably 35~. The operating time is preferably 60 minutes at 55 °C.

In the method for sterilizing powder granules, when the powder granules are gluten-coated egg powder, the weight ratio of the gluten-coated egg powder to the supercritical sterilizing fluid is preferably 1:1.5, wherein the supercritical sterilizing fluid can be selected as a supercritical carbon dioxide fluid containing 0.5% by weight of ethanol and 0.5% of acetic acid, and the operating pressure of the supercritical carbon dioxide fluid is preferably 1500 psi per square inch. The operating temperature is preferably 40 to 55 ° C, and the operating time is preferably 60 minutes.

According to the above technical feature, the sterilizing method for powder granules of the present invention is capable of sterilizing powder granules having heat sensitive components, without Under the influence of the activity of the heat sensitive component, a better bactericidal effect is further achieved.

The above and other objects, features and advantages of the present invention will become more <RTIgt; The method of sterilizing a powder is contacted with a supercritical sterilizing fluid for 20 to 120 minutes, wherein the supercritical sterilizing flow system comprises 0.1-1.0% by weight of ethanol and 0.1-0.5% of acetic acid. The supercritical carbon dioxide fluid has an operating temperature of 40 to 60 ° C and an operating pressure of 1,500 to 3,000 psi per square inch.

The "powder granule" of the present invention contains a food or a drug or the like which is formed into a stacked structure from a powdery or granulated form; for example, a powder containing a physiologically active enzyme or other heat sensitive component, including egg powder, Bacterial powder, Chinese medicinal material powder or pharmacological components and cells covered or preserved with vesicles, but not limited thereto.

More specifically, the supercritical sterilizing flow system of the present invention comprises a supercritical carbon dioxide fluid and a mixed solution of ethanol and acetic acid, wherein the supercritical sterilizing flow system is highly permeable, high in mass, and high in supercritical carbon dioxide fluid. The characteristics of the diffusion coefficient and the low surface tension can enter the dead corners of the powder particles or their stacked structures, and the polar characteristics of the supercritical carbon dioxide fluid are changed by the mixed solution of ethanol and acetic acid. The supercritical sterilizing fluid of the invention can more easily cause damage to the bacterial cells or endospores on the surface of the powder granules, thereby improving the super The bactericidal effect of the carbon dioxide fluid is to destroy the bacterial cells or endospores contained in the powder granules, and to shrink the endospores, thereby further achieving the purpose of comprehensive sterilization.

In the present invention, when the powder granules are in contact with the supercritical sterilizing fluid, it is preferred to contact the powder granules with a fixed weight of the supercritical sterilizing fluid for 20 to 120 minutes to make the powder granules. The cells or the endospores which are present in the substance interact with the supercritical sterilizing fluid. For example, the weight ratio of the powder granules to the supercritical sterilizing fluid is preferably 1:1 to 1:3.

In a preferred embodiment of the present invention, the powder granules are contacted with the supercritical sterilizing fluid in a dynamic sterilizing treatment manner. In particular, when the powder granules are in contact with the supercritical sterilizing fluid, The infusion rate of 20 to 100 ml per minute is supplemented with a new supercritical sterilizing fluid to displace a portion of the supercritical sterilizing fluid that has been exposed to the powder granules. In this way, the supercritical sterilizing fluid can be rendered in a disturbing state, so that the supercritical sterilizing fluid can sufficiently contact the powder granules, and the supercritical sterilizing fluid is ensured to have a better bactericidal effect.

For example, in a practical embodiment of the preferred embodiment of the present invention, a supercritical fluid device as shown in FIG. 1 is provided to sterilize the powder particles, and the supercritical fluid device of the embodiment is The UK-SFE-100-20 type, the supercritical fluid device comprises a carbon dioxide tank, a secondary solvent tank 2 and a sterilization tank 3. The carbon dioxide tank 1 and the auxiliary solvent tank 2 are respectively connected to the sterilization tank. 3.

The carbon dioxide tank 1 is used for accommodating carbon dioxide gas. Preferably, a high pressure pump 11, at least one valve 12, and a back pressure valve are disposed on the communication line between the carbon dioxide tank 1 and the sterilization tank 3. 13 and several hot The exchanger 14 pressurizes the carbon dioxide gas in the carbon dioxide tank 1 with the high pressure pump 11 to become a supercritical carbon dioxide fluid, and controls the supercritical with the high pressure pump 11, the valve 12 and the back pressure valve. The flow rate and direction of the carbon dioxide fluid flowing into the sterilization tank tank 3 are used to control the temperature of the communication line to ensure that the carbon dioxide is in a supercritical state.

The auxiliary solvent tank 2 is used for accommodating a mixed solution of ethanol and acetic acid. Preferably, a pump 21 and at least one valve 22 are disposed on the communication line between the auxiliary solvent tank 2 and the sterilization tank 3. The pump 21 and the valve 22 control the flow rate and direction of the mixed solution of ethanol and acetic acid into the sterilization tank tank 3.

The sterilizing tank 3 has an accommodating space for arranging a powder granule to be sterilized. The sterilizing tank 3 further includes a gate 31, at least one vent valve 32 and a needle valve 33. The space is connected to the external space via the gate 31. The gate 31 is used to close the sterilizing tank 3. The at least one vent valve 32 controls the escape of carbon dioxide gas inside the sterilizing tank 3. The needle valve 33 is The mixed solution of the ethanol and the acetic acid is discharged, and the rear end of the needle valve 33 is connected to a waste liquid tank 34 to hold the mixed solution of the ethanol and the acetic acid; further, the sterilization tank tank 3 is provided with a plurality of heat exchangers 35. In order to control the temperature in the sterilization tank 3, the sterilization tank 3 is further provided with a pressure gauge 36 for the user to confirm the internal pressure of the accommodation space of the sterilization tank 3.

In order to confirm that the sterilizing method for powder granules of the present invention can be applied to the sterilizing treatment of powder granules having a heat sensitive component, the following test was carried out.

Test 1: Supercritical fluid sterilization of green papaya powder

The test provides an array of green papaya powder, and the array of green papaya powder is further mixed with environmental bacteria, and then sterilized by the sterilization method of the invention for powder granules, the environmental flora comprising Escherichia coli , Escherichia coli, yeast or flora that produce endospores and their endospores, etc., but not limited to this; for example, this test is selected by the accession number BCRC 10370 E. coli group, registration number BCRC 10675 is E. coli, the register number BCRC 21812's yeast (Saccharomyces cerevisiae) and the register number BCRC 17530 7.5 log (CFU / g) of Bacillus subtilis (Bacillus atrophaeus) endospores of test Example, and select The array of green papaya powder is dynamically sterilized by a supercritical fluid device as shown in Fig. 1; the supercritical sterilizing flow system of the present embodiment is selected to contain 0.5% by weight of ethanol and 0.5% of acetic acid. The critical carbon dioxide fluid, the weight ratio of the green papaya powder to the supercritical sterilizing fluid is 1:1.5, and the operating pressure of the supercritical carbon dioxide fluid is 1500 psi per square inch Run time was 60 minutes, wherein the operating conditions in order to test the bactericidal effect at different operating temperatures (25 ~ 55 ℃).

Please refer to Figure 2, the X-axis is sterilized at different operating temperatures of 25~55 °C, and the Y-axis is the logarithmic value (Log CFU/g) of each gram of green papaya powder corresponding to each group at different operating temperatures. It can be seen from Fig. 2 that under the dynamic sterilization treatment, when the operating temperature of the supercritical carbon dioxide fluid is 40 to 55 ° C, the sterilization effect of 4 log (CFU/g) or more can be achieved, and at the same time, the papaya in the green papaya powder The enzyme is not inactivated by the destruction of the supercritical sterilizing solution.

In addition, please refer to Figures 3 and 4 again for the endospore The above conditions are shown in the electro-photographs before and after sterilization. It can be clearly seen from the third and fourth figures that the sterilization conditions of the present embodiment can cause the endospores to shrink and make them less susceptible to germination, confirming the operation of the present embodiment. The activity of reducing endospores can be achieved.

Test 2: Supercritical fluid sterilization of micro-lipid coated egg powder

The experiment provides an array of micro-lipid coated egg powder, and the array of micro-lipid coated egg powder is further mixed with the environmental flora, and then sterilized by the sterilization method of the invention for powder granules, The environmental flora contains Escherichia coli, Escherichia coli, Salmonella, yeast or flora that produces endospores and their endospores, but not limited thereto; for example, this experiment is selected by the registration number. The Escherichia coli group of BCRC 10370, Escherichia coli with accession number BCRC 10675, yeast ( Saccharomyces cerevisiae ) with accession number BCRC 21812, Salmonella typhimurium with accession number BCRC12949, and 7.5 log with accession number BCRC 17530 ( CFU/g) Bacillus atrophaeus endophytes were used as test examples, and the supercritical fluid device as shown in Fig. 1 was selected to dynamically sterilize the array of microlipid coated egg powder; The supercritical sterilizing flow system of the embodiment is selected as a supercritical carbon dioxide fluid containing 0.5% by weight of ethanol and 0.5% of acetic acid, and the aliquot is coated with egg powder and the The weight ratio of the critical sterilizing fluid is 1:1.5, the operating pressure of the supercritical carbon dioxide fluid is 1500 psi per square inch, and the operation time is 60 minutes, wherein different operating temperatures (25-55 ° C) are tested under the aforementioned operating conditions. The bactericidal effect.

Please refer to Figure 5, the X-axis system is sterilized at different operating temperatures of 25~55 °C. The Y-axis is the corresponding per gram of micro-fat at different operating temperatures. The logarithmic value of log coated egg powder (Log CFU / g), as shown in Figure 5, under the dynamic sterilization treatment, the operating temperature of the supercritical carbon dioxide fluid is 40 ~ 55 ° C, can reach 4 log (CFU / g) The above bactericidal effect, at the same time, the liposome-coated egg powder contains chicken ovomucoid protein (CHOM), a specific inhibitor of trypsin, which was identified as an average of 17.08 mg. /mL, tested to verify that more than 70% inhibition of trypsin inhibition activity, indicating that CHOM is not destroyed by the destruction of the supercritical sterilization solution.

It can be seen that the present invention can indeed sterilize the powder granules to improve the contamination of the powder granules by microorganisms in the environment, such as Escherichia coli, Escherichia coli, Salmonella, yeast or Bacillus. The spores and the like can be surely reduced in the amount of microorganisms contained therein by the method of the present invention without destroying the heat sensitive component in the powder granules.

Thereby, the sterilizing method for powder granules of the present invention can achieve the effect of improving the bactericidal effect of various powder granules without affecting the activity conditions of the various powder granules.

The sterilizing method for powder granules of the invention is capable of removing bacteria, molds or spores contaminated on the surface of the powder granules, and reducing the number of environmental microorganisms which are noisy in various powder granules, so as to improve The efficacy of the bactericidal effect of various powder granules.

While the invention has been described in connection with the preferred embodiments described above, it is not intended to limit the scope of the invention. The technical scope of the invention is protected, and therefore the scope of the invention is defined by the scope of the appended claims.

1‧‧‧CO2 tank

11‧‧‧High pressure pump

12‧‧‧ Valve

13‧‧‧Back pressure valve

14‧‧‧ heat exchanger

2‧‧‧Secondary solvent tank

21‧‧‧ pump

22‧‧‧ Valve

3‧‧‧Sterilization tank

31‧‧‧ gate

32‧‧‧Discharge valve

33‧‧‧needle valve

34‧‧‧ Waste tank

35‧‧‧ heat exchanger

36‧‧‧ Pressure gauge

Figure 1 is a diagram showing the piping configuration of a supercritical fluid device according to a preferred embodiment of the present invention.

Fig. 2 is a line diagram showing the sterilization rate of each environmental flora of Test 1 of the present invention.

Fig. 3 is a diagram showing the appearance of endospores before sterilization by the test of the present invention.

Fig. 4 is a diagram showing the appearance of endospore after sterilization by the test of the present invention.

Fig. 5 is a line diagram showing the sterilization rate of each environmental flora of the second test of the present invention.

1‧‧‧CO2 tank

11‧‧‧High pressure pump

12‧‧‧ Valve

13‧‧‧Back pressure valve

14‧‧‧ heat exchanger

2‧‧‧Secondary solvent tank

21‧‧‧ pump

22‧‧‧ Valve

3‧‧‧Sterilization tank

31‧‧‧ gate

32‧‧‧Discharge valve

33‧‧‧needle valve

34‧‧‧ Waste tank

35‧‧‧ heat exchanger

36‧‧‧ Pressure gauge

Claims (13)

A method for sterilizing powder granules by contacting the powder granules with a supercritical sterilizing fluid for 20 to 120 minutes, wherein the supercritical sterilizing stream system contains 0.1% to 1.0% by weight of ethanol And a supercritical carbon dioxide fluid of 0.1 to 0.5% acetic acid, the operating temperature of the supercritical carbon dioxide fluid is 40 to 60 ° C, and the operating pressure is 1500 to 3000 pounds per square inch. The sterilizing method for powder granules according to claim 1, wherein the powder granules and the supercritical sterilizing when the powder granules are in contact with a supercritical sterilizing fluid The weight ratio of the fluid is 1:1~1:3. The sterilizing method for powder granules according to claim 1 or 2, wherein the powder granules are in contact with the supercritical sterilizing fluid, and the powder is dynamically sterilized. The granules are contacted with the supercritical sterilizing fluid, which is supplemented with a new supercritical sterilizing fluid at an infusion rate of 20 to 100 ml per minute to displace a portion of the supercritical sterilizing fluid that has been contacted with the granules of the powder. The bactericidal method for powder granules according to claim 1, wherein the powder granule is green papaya powder, and the weight ratio of the green papaya powder to the supercritical sterilizing fluid is 1: 1.5. The sterilizing method for powder granules according to claim 4, wherein the supercritical sterilizing fluid system comprises a supercritical carbon dioxide fluid having 0.5% by weight of ethanol and 0.5% of acetic acid. Sterilization for powder granules as described in claim 5 The method wherein the supercritical carbon dioxide fluid is operated at a pressure of 1500 pounds per square inch. The sterilizing method for powder granules according to claim 6, wherein the supercritical carbon dioxide fluid has an operating temperature of 40 to 55 °C. The sterilizing method for powder granules according to claim 7, wherein the supercritical carbon dioxide fluid has an operation time of 60 minutes. The sterilizing method for powder granules according to claim 1, wherein the powder granule is a gluten-coated egg powder, and the gluten-coated granule powder and the supercritical The weight ratio of the sterilizing fluid is 1:1.5. The sterilizing method for powder granules according to claim 9, wherein the supercritical sterilizing fluid system comprises a supercritical carbon dioxide fluid of 0.5% by weight of ethanol and 0.5% of acetic acid. The sterilizing method for powder granules according to claim 10, wherein the supercritical carbon dioxide fluid has an operating pressure of 1,500 psi per square inch. The sterilizing method for powder granules according to claim 11, wherein the supercritical carbon dioxide fluid has an operating temperature of 40 to 55 °C. The sterilizing method for powder granules according to claim 12, wherein the supercritical carbon dioxide fluid has an operation time of 60 minutes.