CN114264633B - Formalin polymer freeze-dried powder and preparation method thereof - Google Patents
Formalin polymer freeze-dried powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a formalin polymer freeze-dried powder and a preparation method thereof, wherein a freeze vacuum drying technology of adding freeze-drying excipient is adopted to prepare formalin polymer into the formalin polymer freeze-dried powder, and the storage stability of the formalin polymer freeze-dried powder is obviously improved relative to formalin polymer turbidity standard liquid; particularly, the low-concentration formalin polymer turbidity standard solution can be prepared into a quantified formalin polymer freeze-dried powder finished product, when the low-concentration formalin polymer turbidity standard solution is required to be used, the quantified formalin polymer freeze-dried powder is only required to be added into a certain amount of re-dissolving solution for re-dissolving, the operation is convenient, and the practicability is high. The formalin polymer freeze-dried powder prepared by the preparation method of the formalin polymer freeze-dried powder disclosed by the invention is high in stability, convenient to store and transport, good in redissolution property and convenient to operate, and is beneficial to improving the working efficiency in water turbidity detection.
Description
Technical Field
The invention relates to the technical field of water quality detection, and particularly relates to formalin polymer freeze-dried powder and a preparation method thereof.
Background
Turbidity measurements, which are important as indicators of water quality, are a measure of the decrease in transparency of a liquid due to the presence of colloidal particles in the water that scatter and absorb visible light. The turbidity measurement methods are generally classified into: nephelometry, visual turbidimetry, spectrophotometry, among which nephelometry is widely used for the determination of turbidity of water quality because of its rapid measurement and easy operation, and is also a turbidimetry prescribed by the standardization group (ISO) and the Environmental Protection Agency (EPA). The nephelometry specifically comprises: a beam of stable light source is utilized to pass through a sample cell containing a sample to be measured, a sensor is positioned at a position vertical to incident light to measure the intensity of scattered light, and the ratio of the intensity of the scattered light to the intensity of the incident light at the vertical position is in a direct proportion relation with the turbidity of the sample within a certain concentration range.
The national environmental protection standard, "turbidity determination for water turbidity", published by the ministry of ecological environment (HJ1075-2019) accepts formalin as the main standard for turbidity detection in water. According to ISO standard 7027:1999, the preparation of the standard liquid related to water turbidity is that the preparation of the standard liquid of formalin requires equal volume mixing of 100g/L hexamethylenetetramine solution and 10g/L hydrazine sulfate solution, and the mixture is kept at 25 ℃ for 24h to generate condensation reaction to form insoluble white aqueous formalin polymer suspension, so as to prepare a turbidity standard stock solution with the turbidity of 4000NTU, and the turbidity standard stock solution can be preserved in the dark for 6 months at room temperature; when the high-concentration formalin standard stock solution is diluted to 400NTU by using zero-concentration water, the formalin standard stock solution can be refrigerated at 4 ℃ and stored in a dark place for 1 month; when a standard stock solution of high-concentration formalin is diluted to 0-100NTU by using zero-degree water, the standard solution of the formalin needs to be prepared immediately, because the standard solution of the formalin with low concentration is easy to degrade quickly.
US patent US 5777011a filed by hash corporation in 1995 discloses a stabilized formalin polymer suitable as a turbidity standard which can be prepared by diluting an aqueous formalin raw material composition having a turbidity of more than 400NTU with a diluent containing hexamethylenetetramine and optionally a water-soluble sulfate salt such as sodium sulfate. The pH of the stabilized formalin polymer should be in the range of about 7-11. Specifically, the pH of the solution is increased by using hexamethylenetetramine or other alkali with the concentration of 50-200 g/L to stabilize the stability of the formalin polymer in the aqueous solution. Although US 5777011a requires that a stabilized formalin polymer solution having turbidity of less than 400NTU remains stable for more than a year, it was found that slow degradation still occurs at low NTU values. In addition, the use of hexamethylenetetramine solutions at concentrations above 50g/L leads to a significant change in the refractive index, which leads to an unstable haze reading.
European Union patent EP3190155A1 and International PCT patent WO2017121575A1, which were filed by German colorimeter Co., Ltd.2017, propose that the key of the stability of the formalin polymer is to prevent pH shift, and propose that the pH of the formalin polymer is adjusted to be within the range of 8.4-10 by using a strategy of a buffer solution system, so that the dosage of hexamethylenetetramine is remarkably reduced to 4g/L to eliminate the refractive index change of a dilution error, and the long-term stability of the formalin polymer is ensured. Based on the buffer solution system, the formalin polymer standard solution with the turbidity of 0.05NTU can still maintain the stability of 12-18 months.
As shown in the chemical reaction equation for preparing the formalin polymer shown in the attached figure 1, the hydrogen ions obtained by hydrolyzing the formalin polymer with hydrazine sulfate hydrolyze hexamethylenetetramine to release formaldehyde, and the formaldehyde is condensed with hydrazine to generate the formalin polymer and water molecules. Based on the luxatel equilibrium principle, the reversible reaction of the obtained formalin polymer and water molecules can push the formalin polymer to be degraded. Because the low-concentration formalin standard solution has more water content compared with the high-concentration formalin solution, the degradation rate of the low-concentration formalin polymer standard solution is higher, and the high-concentration formalin solution has longer stability.
The traditional material drying method is to dry food by heating water to be in a vapor state under a liquid state, and the freezing vacuum drying technology is to utilize the ice crystal sublimation principle to directly sublimate frozen moisture of the material from ice solid to steam under a vacuum environment without melting ice. The freeze vacuum drying technology has the advantages of capability of maintaining sample properties, good re-solubility, less loss of volatile components in the sample when the sample is dried at low temperature, and the like, is commonly used for producing temperature sensitive samples such as penicillin, and is expanded to bioengineering, medical preparations, food industry and the like. Korean patent and international PCT patent No. WO2016108534a1, filed by the drug manufacturing institute of sansho corporation, 2016, propose a freeze-dried polymer nanoparticle aqueous solution comprising an amphiphilic block copolymer, a polylactic acid derivative having a carboxyl terminal group, and a freeze-drying aid, and a method for preparing the same.
Freeze-vacuum drying is a complex phase transition process, and in the processes of freezing, freeze-thawing, drying and storage, various factors inducing protein denaturation in the medicine exist, so some measures are often taken to stabilize polymers or proteins in the prescription, and the currently generally adopted method is to add a freeze-drying excipient. The freeze-drying excipient has various types and mechanisms, common freeze-drying excipients comprise polyhydroxy compounds, amino acids, polymers and the like, and the selection of a proper freeze-drying excipient has great significance on the quality stability and the redissolution repeatability in the storage and transportation processes of a freeze-dried product.
At present, no related report of preparing the formalin polymer freeze-dried powder by adding a freeze-drying excipient and adopting a freeze-vacuum drying technology exists. The invention discloses a freeze-vacuum drying technology based on freeze-drying excipient addition, which aims to completely remove water in a formalin solution, fully inhibit hydrolysis reaction of a formalin polymer and water molecules and prepare the formalin polymer freeze-dried powder with good stability.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a preparation method of formalin polymer freeze-dried powder, wherein the formalin polymer is prepared into the formalin polymer freeze-dried powder by adopting a freeze vacuum drying technology of adding a freeze-drying excipient, and the formalin polymer freeze-dried powder obviously improves the storage stability relative to formalin polymer turbidity standard solution; particularly, the low-concentration formalin polymer turbidity standard solution can be prepared into a quantified formalin polymer freeze-dried powder finished product, when the low-concentration formalin polymer turbidity standard solution is required to be used, the quantified formalin polymer freeze-dried powder is only required to be added into a certain amount of re-dissolving solution for re-dissolving, the operation is convenient, and the practicability is high. The formalin polymer freeze-dried powder prepared by the preparation method of the formalin polymer freeze-dried powder disclosed by the invention is high in stability, convenient to store and transport and good in redissolution property, only a certain amount of redissolution needs to be added into the quantified formalin polymer freeze-dried powder for redissolution, the operation is convenient, and the work efficiency in water turbidity detection is improved.
In order to achieve the above purpose, one of the purposes of the present invention is to design a preparation method of formalin polymer freeze-dried powder, which comprises the following operation steps:
s1: drying solid powder of hexamethylenetetramine and solid powder of hydrazine sulfate, then weighing a certain mass of dried hexamethylenetetramine powder and hydrazine sulfate powder, and respectively dissolving the weighed hexamethylenetetramine powder and hydrazine sulfate powder in deionized water, wherein the mass ratio of the hexamethylenetetramine powder to the hydrazine sulfate powder is 10: 1, so as to obtain hexamethylenetetramine aqueous solution and hydrazine sulfate aqueous solution;
s2: mixing the hexamethylenetetramine aqueous solution and the hydrazine sulfate aqueous solution prepared in the step S1, uniformly stirring, and then placing for more than 24 hours at the temperature of 22-28 ℃ to obtain a formalin polymer solution;
s3: adding a certain amount of freeze-drying excipient into the formalin polymer solution prepared in the step S2, adding an inorganic alkali solution to adjust the pH to 8.5-10, and uniformly stirring to form a formalin polymer suspension;
s4: and (5) sequentially pre-freezing and freezing, sublimation drying and resolution drying the formalin polymer suspension prepared in the step S3 to obtain a finished product of the formalin polymer freeze-dried powder.
Preferably, in step S3, the addition amount of the freeze-drying excipient is 10 wt% -20 wt% of the weight of the hexamethylenetetramine powder weighed in step S1, and the inorganic alkali solution is one of a sodium hydroxide aqueous solution, a potassium hydroxide aqueous solution and a strong base and weak acid salt aqueous solution.
Further preferably, the freeze-drying excipient is any one or more of mannitol, sorbitol, maltitol, xylitol, lactitol, arginine and glycine.
Further preferably, in step S4, the pre-freezing operation is: freezing the formalin polymer suspension prepared in the step S3 to-40 ℃ within 30min, and keeping the formalin polymer suspension at-40 ℃ for 1-3 h to obtain a pre-frozen product;
the specific operation of sublimation drying is as follows: heating the pre-frozen product to-30 ℃ at the speed of 10 ℃/h, then heating to-20 ℃ at the speed of 5 ℃/h, and keeping the temperature at-20 ℃ for 5-8 h to obtain a primary dried product;
the specific operation of the analysis and drying is as follows: heating the primary dried product to-10 ℃ at the speed of 10 ℃/h, heating to 0 ℃ at the speed of 10 ℃/h, heating to 10 ℃ at the speed of 5 ℃/h, and heating to 20 ℃ at the speed of 2 ℃/h to obtain the finished product of the formalin polymer freeze-dried powder.
Further preferably, in the step S4, the temperature reduction speed in the pre-freezing and cooling process is more than or equal to 2 ℃/min.
The second purpose of the invention is to design a formalin polymer freeze-dried powder which is prepared by adopting the preparation method of the formalin polymer freeze-dried powder.
The invention has the advantages and beneficial effects that:
1. the invention discloses a preparation method of formalin polymer freeze-dried powder, which is characterized in that formalin polymer is prepared into formalin polymer freeze-dried powder by adopting a freeze vacuum drying technology of adding freeze-drying excipient, and the formalin polymer freeze-dried powder obviously improves the storage stability relative to formalin polymer turbidity standard liquid; particularly, the low-concentration formalin polymer turbidity standard solution can be prepared into a quantified formalin polymer freeze-dried powder finished product, when the low-concentration formalin polymer turbidity standard solution is required to be used, the quantified formalin polymer freeze-dried powder is only required to be added into a certain amount of re-dissolving solution for re-dissolving, the operation is convenient, and the practicability is high.
2. The formalin polymer freeze-dried powder prepared by the preparation method of the formalin polymer freeze-dried powder is used as a turbidity standard liquid precursor, is high in stability, convenient to store and transport and good in redissolution property, only needs to be added with a certain amount of redissolution for redissolution, is convenient to operate, and is beneficial to improving the working efficiency during water turbidity detection.
3. The formalin polymer freeze-dried powder prepared by the method for preparing the formalin polymer freeze-dried powder is taken at any time, and compared with a turbidity calibration method for sampling after quantitatively diluting a high-turbidity formalin standard solution which is prepared at present in the prior art, the method effectively improves the utilization rate of the formalin polymer to 100%.
Drawings
FIG. 1 is a chemical reaction equation for formalin polymer;
fig. 2 is a transmission electron micrograph of the formalin polymer obtained after redissolving the formalin polymer lyophilized powder prepared in example 2.
Detailed Description
The following description of the embodiments of the present invention will be made with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1
The invention discloses a formalin polymer freeze-dried powder which is prepared by adopting a preparation method of the formalin polymer freeze-dried powder, and the preparation method comprises the following operation steps:
s1: preparing a hexamethylenetetramine aqueous solution and a hydrazine sulfate aqueous solution, respectively spreading hexamethylenetetramine solid powder and hydrazine sulfate solid powder on a watch glass, placing the watch glass in a silica gel dryer for 48 hours to remove wet water, then weighing 50g (accurate to 0.01g) of dried hexamethylenetetramine powder and 5g (accurate to 0.01g) of dried hydrazine sulfate powder, and respectively dissolving the hexamethylenetetramine powder and the hydrazine sulfate powder in 400mL of deionized water to obtain a hexamethylenetetramine aqueous solution and a hydrazine sulfate aqueous solution;
s2: preparing 4000NTU turbidity formalin polymer standard solution, combining the hexamethylenetetramine aqueous solution and the hydrazine sulfate aqueous solution prepared in the step S1, transferring the combined solution into a 1000mL volumetric flask, fixing the volume to a marked line, and then placing the volumetric flask at the temperature of 25 ℃ for 24 hours to induce the hexamethylenetetramine and the hydrazine sulfate to condense to generate the formalin polymer so as to obtain the 4000NTU turbidity formalin polymer standard solution;
s3: adding 10g of sorbitol (freeze-drying excipient) into the formalin polymer solution prepared in the step S2, adjusting the pH to 9.5 by using 1mol/L potassium hydroxide aqueous solution, and uniformly stirring to form a formalin polymer suspension;
s4: and (5) sequentially pre-freezing and freezing, sublimation drying and resolution drying the formalin polymer suspension prepared in the step S3 to obtain a finished product of the formalin polymer freeze-dried powder.
Preferably, in step S4, the pre-freezing operation is: freezing the formalin polymer suspension prepared in the step S3 to-40 ℃ within 30min, and keeping the temperature for 2h at-40 ℃ to obtain a pre-frozen product;
the specific operation of sublimation drying is as follows: heating the pre-frozen product to-30 ℃ at the speed of 10 ℃/h, then heating to-20 ℃ at the speed of 5 ℃/h, and keeping the temperature for 5h at the temperature of-20 ℃ to obtain a primary dried product;
the specific operation of the analysis and drying is as follows: heating the primary dried product to-10 ℃ at the speed of 10 ℃/h, heating to 0 ℃ at the speed of 10 ℃/h, heating to 10 ℃ at the speed of 5 ℃/h, and heating to 20 ℃ at the speed of 2 ℃/h to obtain the finished product of the formalin polymer freeze-dried powder.
Further preferably, in the step S4, the temperature reduction speed in the pre-freezing and cooling process is more than or equal to 2 ℃/min.
Example 2
A quantified finished product of formalin polymer freeze-dried powder is prepared by the preparation method of the formalin polymer freeze-dried powder, and comprises the following operation steps:
h1: preparing a hexamethylenetetramine aqueous solution and a hydrazine sulfate aqueous solution, respectively paving hexamethylenetetramine solid powder and hydrazine sulfate solid powder on a watch glass, placing the watch glass in a silica gel dryer for 48 hours to remove wet water, then weighing 5.0g (accurate to 0.01g) of dried hexamethylenetetramine powder and 0.5g (accurate to 0.01g) of dried hydrazine sulfate powder, and respectively dissolving the hexamethylenetetramine powder and the hydrazine sulfate powder in 40mL of deionized water to obtain a hexamethylenetetramine aqueous solution and a hydrazine sulfate aqueous solution;
h2: preparing a 4000NTU turbidity elmazi polymer standard solution, combining the hexamethylenetetramine aqueous solution and the hydrazine sulfate aqueous solution prepared in the step S1, transferring the combined solution into a 100mL volumetric flask, fixing the volume to a marked line, and then placing the volumetric flask at the temperature of 22 ℃ for 26 hours to induce the hexamethylenetetramine and the hydrazine sulfate to condense to generate a formalin polymer so as to obtain the 4000NTU turbidity formalin polymer standard solution;
h3: subpackaging the formalin polymer suspension, transferring a certain amount of the formalin polymer standard solution prepared in the step H2 into a penicillin bottle according to the turbidity value of the formalin polymer standard solution to be prepared, adding 0.5g of mannitol (freeze-drying excipient) into the penicillin bottle, adjusting the pH value to 8.5 by using 0.1mol/L sodium hydroxide aqueous solution, and uniformly stirring to form quantitative formalin polymer suspension;
considering that the concentration C and the turbidity T of the formalin polymer suspension are in a linear proportion positive correlation in a certain range, according to a calculation formula
The definitions and units of the parameters in the formula are as follows:
| symbols of formulas | Chemical significance | Unit of |
| V stock | Volume of solution removed from turbidity Standard stock solution | mL |
| T stock | Turbidity Standard the turbidity of the stock solution (here 4000NTU) | NTU |
| V reconstitution | Standard water amount for redissolution | mL |
| T reconstitution | Theoretical turbidity of turbidity standard solution obtained after redissolution | NTU |
Standard water volume V for redissolution reconstitution Taking 20mL, taking turbidity check points such as 1NTU, 20NTU, 200NTU, 1000NTU, 4000NTU, etc., and polymerizing formalin under 4000NTU turbidityOn the basis of the standard solution, the following 4000NTU turbidity formalin polymer standard solution is properly transferred into a penicillin bottle,
| recommending a calibration point T reconstitution | Moving V stock |
| 4000NTU | 20mL |
| 1000NTU | 5mL |
| 200NTU | 1mL |
| 20NTU | 0.1mL |
| 1NTU | 5uL |
Standard water volume V for redissolution reconstitution Taking 500mL, taking turbidity check points of 0.1NTU, 2NTU, 20NTU, 200NTU and the like, properly transferring 4000NTU turbidity formalin polymer standard solution with the following volume into a penicillin bottle on the basis of the 4000NTU turbidity formalin polymer standard solution,
| recommending a calibration point T reconstitution | Moving V stock |
| 200NTU | 25mL |
| 20NTU | 2.5mL |
| 2NTU | 0.25mL |
| 0.1NTU | 12.5uL |
H4: pre-freezing the frozen formalin polymer suspension, freezing a penicillin bottle containing the quantitative formalin polymer suspension in the step H3 to-40 ℃ within 30min, and keeping the penicillin bottle at the temperature of-40 ℃ for 3H to obtain a pre-frozen product;
heating the pre-frozen product to-30 ℃ at the speed of 10 ℃/h, then heating to-20 ℃ at the speed of 5 ℃/h, and keeping the temperature at-20 ℃ for 8h to obtain a primary dried product;
heating the primary dried product to-10 ℃ at the speed of 10 ℃/h, heating to 0 ℃ at the speed of 10 ℃/h, heating to 10 ℃ at the speed of 5 ℃/h, and heating to 20 ℃ at the speed of 2 ℃/h to obtain the formalin polymer freeze-dried powder which is fully dried and has loose texture;
h5: and (5) bottling and labeling, namely, capping and labeling the penicillin bottle containing the formalin polymer freeze-dried powder prepared in the step H4 to obtain a quantified finished product of the formalin polymer freeze-dried powder.
Preparing the formalin polymer freeze-dried powder finished product quantified by other specifications according to the steps H1-H5, and when the quantified formalin polymer freeze-dried powder finished product is used, only a certain amount of redissolution needs to be added into a penicillin bottle, and the penicillin bottle is shaken to fully dissolve the formalin polymer, so that the formalin polymer turbidity standard solution with a standard turbidity value is formed. Wherein, the finished product of the quantified formalin polymer freeze-dried powder prepared in the embodiment 2 is added with filtered water with turbidity value smaller than the detection limit obtained by filtering through a microporous filter membrane with the pore diameter smaller than 0.45 μm to be re-dissolved into the formalin polymer turbidity standard solution, and a transmission electron microscope photo of the turbidity standard solution is shown in fig. 2. As can be seen from fig. 2, the morphological feature of the formalin polymer in the formalin polymer turbidity standard solution after redissolving is consistent with the morphological feature of the formalin polymer in the formalin polymer turbidity of 4000NTU in step H2, which indicates that the formalin polymer freeze-dried powder prepared by the method of the present invention has high stability and good redissolution performance, and the object of the present invention is achieved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the technical principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. The preparation method of the formalin polymer freeze-dried powder is characterized by comprising the following operation steps:
s1: drying solid powder of hexamethylenetetramine and solid powder of hydrazine sulfate, then weighing a certain mass of dried hexamethylenetetramine powder and hydrazine sulfate powder, and respectively dissolving the weighed hexamethylenetetramine powder and hydrazine sulfate powder in deionized water, wherein the mass ratio of the hexamethylenetetramine powder to the hydrazine sulfate powder is 10: 1, so as to obtain hexamethylenetetramine aqueous solution and hydrazine sulfate aqueous solution;
s2: mixing the hexamethylenetetramine aqueous solution and the hydrazine sulfate aqueous solution prepared in the step S1, uniformly stirring, and then placing for more than 24 hours at the temperature of 22-28 ℃ to obtain a formalin polymer solution;
s3: adding a certain amount of freeze-drying excipient into the formalin polymer solution prepared in the step S2, adding an inorganic alkali liquor to adjust the pH to 8.5-10, and uniformly stirring to form a formalin polymer suspension, wherein the freeze-drying excipient is any one or more of mannitol, sorbitol, maltitol, xylitol, lactitol, arginine and glycine, and the inorganic alkali liquor is one of a sodium hydroxide aqueous solution, a potassium hydroxide aqueous solution and a strong alkali and weak acid salt aqueous solution;
s4: and (5) sequentially pre-freezing and freezing, sublimation drying and resolution drying the formalin polymer suspension prepared in the step S3 to obtain a finished product of the formalin polymer freeze-dried powder.
2. The method for preparing formalin polymer lyophilized powder as claimed in claim 1, wherein in step S3, the addition amount of the lyophilized excipient is 10 wt% -20 wt% of the weight of the hexamethylenetetramine powder weighed in step S1.
3. The method for preparing formalin polymer lyophilized powder as claimed in claim 1, wherein in step S4, the pre-freezing operation is: freezing the formalin polymer suspension prepared in the step S3 to-40 ℃ within 30min, and keeping the formalin polymer suspension at-40 ℃ for 1-3 h to obtain a pre-frozen product;
the specific operation of sublimation drying is as follows: heating the pre-frozen product to-30 ℃ at the speed of 10 ℃/h, then heating to-20 ℃ at the speed of 5 ℃/h, and keeping the temperature at-20 ℃ for 5-8 h to obtain a primary dried product;
the specific operation of the analysis and drying is as follows: heating the primary dried product to-10 ℃ at the speed of 10 ℃/h, heating to 0 ℃ at the speed of 10 ℃/h, heating to 10 ℃ at the speed of 5 ℃/h, and heating to 20 ℃ at the speed of 2 ℃/h to obtain the finished product of the formalin polymer freeze-dried powder.
4. The method for preparing the formalin polymer freeze-dried powder as claimed in claim 3, wherein in the step S4, the temperature reduction speed in the pre-freezing and freezing temperature reduction process is not less than 2 ℃/min.
5. A formalin polymer freeze-dried powder characterized by being prepared by the preparation method of the formalin polymer freeze-dried powder according to any one of claims 1-4.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US5777011A (en) * | 1995-12-01 | 1998-07-07 | Hach Company | Stabilized formazin composition |
| EP3190155B1 (en) * | 2016-01-11 | 2018-03-14 | Tintometer GmbH | Stabilised formazin composition, method of preparation and diluent for formazin composition |
| US10006853B2 (en) * | 2016-10-25 | 2018-06-26 | Hach Company | Vial and cap for turbidity standard |
| AU2020204922A1 (en) * | 2019-01-06 | 2021-07-01 | Endo Global Aesthetics Limited | Collagenase formulations and methods of producing the same |
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